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At least 271 records · Page 15

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DOE OSTI2024

Phase field modeling of hydrogen release in nitrile-butadiene rubber composites after high-pressure hydrogen exposure

Experimental data showed that a simple diffusion model doesn’t suffice to explain the hydrogen (H 2 ) release kinetics in nitrile butadiene rubber (NBR) composites (one with no filler or plasticizer, one with plasticizer only, one with fillers and plasticizer, and one with fillers only) after exposed to hydrogen gas at a pressure of 27.6 MPa. In this work, we developed a phase field model that considers the effect of H 2 gas bubble evolution on H 2 release kinetics. With the model, we simulated the effect of thermodynamic and kinetics properties on the nucleation, growth, and shrinkage of gas bubbles and H 2 release kinetics during and after decompression. Here, the results demonstrated that 1) the model built upon certain thermodynamic and kinetics properties of a given material can well describe its H 2 release kinetics measured in experiments, and 2) the model can predict the gas bubble evolution, which is associated with the material property degradation and failures, with accurate thermodynamic and kinetics properties or H 2 release data from experiments.

08 HYDROGEN↗

DOE OSTI2022

Quantitative assessment of particle dispersion in polymeric composites and its effect on mechanical properties

In this work, an automated image analysis tool is developed to establish quantitative correlations between the particle/cluster size distribution and the mechanical properties of particle reinforced polymer composites (PRPC).This automated image analysis tool is developed within python programming software to process and analyze the microstructural images of the polymerbased composite materials. The spent coffee bean powder (SCBP) reinforced poly-propylene carbonate (PPC) polymer composite with differing wt.% of the filler is selected for the analysis. Detailed statistical analysis of the microstructural images reveals that ‘clustering of clusters’ is also presented in addition to the most commonly reported ‘clustering of particles’, and the distribution of particle/clusters is bimodal. Based on these findings, an effective volume fraction for the filler material is proposed to mainly capture the agglomeration effect. With this effective volume fraction, the standard rule-of-mixture model correctly captures the experimentally measured tensile strength and modulus as a function of filler wt.%. Further, the applicability of this effective volume fraction for other theoretical models is also analyzed. The detailed statistical analysis of the microstructure and the proposed effective volume fraction helps to develop a deeper quantitative understanding of the PRPC than the conventional qualitative correlation of microstructural features with the properties and failure processes.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Critical role of polymer-ceramic ion exchange for high conductivity composite electrolytes

Polymer-ceramic composites offer a path to enhance the transport and mechanical properties of solid electrolytes. However, an in-depth understanding of the extent and role of ion transport along and across polymer-ceramic interfaces in these systems is lacking. We have recently shown that Li-conducting Li 0.11 Na 0.24 K 0.02 La 0.43 TiO 2.82 (LMTO) nanorods can be prepared by a molten flux method, and the addition of 30–50 weight (wt.)% LMTO to a bis[(trifluoromethyl)sulfonyl]imide-vinyl ethylene carbonate-based single-ion conducting (SIC) polymer electrolyte leads to a two-fold enhancement in Li-ion conductivity, from 1.4 to 3.0 × 10 −5 S/cm at 30 °C. In the present study, we use NMR methods to identify the Li-ion transport pathways and determine the timescale of chemical exchange between the SIC polymer and LMTO ceramic components. Tracer exchange NMR indicates preferential transport through the polymer or polymer-interfacial regions, and exchange spectroscopy (EXSY) and a new isotope exchange method reveal negligible Li exchange between the SIC polymer and LMTO ceramic up to several days. Here, LMTO nanorods act as a passive filler. Our results further highlight that significant (e.g., 10- or 100-fold) conductivity enhancements in composite electrolytes can only be achieved 1) with ionically-conductive fillers, and 2) when both the ceramic and polymer components actively participate in long-range transport. For this, fast interfacial ion exchange is needed. In conclusion, this leads us to introduce a critical interfacial ion exchange time to evaluate whether a filler actively contributes to conduction in a composite electrolyte, and screen for promising polymer-ceramic pairings to accelerate the development of high conductivity solid electrolytes.

Battery, Solid electrolyte↗

DOE OSTI2026

Effects of PLA/PHB Blend Ratio and Wood Flour Loading on the Melt Rheology and Thermomechanical Properties of Biobased Polymer Composites

The development of sustainable, biobased polymer composites is crucial for reducing supply chain dependence on fossil fuels. A major challenge lies in understanding and predicting the processability of these sustainable material alternatives, which directly impacts large-scale manufacturing. Here, this study systematically investigates the effect of poly(lactic acid) (PLA)/polyhydroxybutyrate (PHB) blend ratios and wood flour (WF) loadings on the thermal, rheological, and mechanical properties of the composites. Composites were prepared via melt compounding and characterized by using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), oscillatory shear melt rheology, tensile testing, and scanning electron microscopy. Results showed that increasing the PHB content lowered the glass transition temperature, while higher PHB and WF loadings decreased thermal stability. Complex viscosity decreased with increasing PHB in 0 and 10% WF, whereas it increased in 20% and 30% WF for PHB-rich blends (80/20 and 70/30 PLA/PHB) due to stronger filler interactions with flexible PHB chains. At 30% WF, PHB-containing composites also showed elastic dominance with G′ higher than G″. This behavior was confirmed by van Gurp–Palmen plots, where the phase angle decreased with increasing PHB and WF loadings. WF addition also shifted Cole–Cole plots away from semicircular terminal relaxation, while time–temperature superposition validity was maintained, confirming that polymer chain dynamics continue to dominate melt behavior. Young’s modulus increased with WF loading, while tensile strength and toughness decreased due to weaker interfacial adhesion between the matrix and the filler. Interestingly, 10% WF systems containing PHB exhibited the highest toughness among all of the filled systems, indicating synergistic reinforcement from WF fillers and PHB-induced ductility. Overall, melt rheology effectively captured the internal structure and stiffness of the composites as the formulation changed, reinforcing the concept that the PLA/PHB ratio and WF content can be tuned to adjust melt elasticity and balance mechanical property trade-offs for targeted applications.

melt rheology↗

DOE OSTI2023

Leveraging peptide–cellulose interactions to tailor the hierarchy and mechanics of peptide–polymer hybrids

Inspired by spider silk's hierarchical diversity, we leveraged peptide motifs with the capability to tune structural arrangement for controlling the mechanical properties of a conventional polymer framework. The addition of nanofiller with hydrogen bonding sites was used as another pathway towards hierarchical tuning via matrix–filler interactions. Specifically, peptide–polyurea hybrids (PPUs) were combined with cellulose nanocrystals (CNCs) to develop mechanically-tunable nanocomposites via tailored matrix–filler interactions (or peptide–cellulose interactions). In this material platform, we explored the effect of these matrix–filler interactions on the secondary structure, hierarchical ordering, and mechanical properties of the peptide hybrid nanocomposites. Interactions between the peptide matrix and CNCs occur in all of the PPU/CNC nanocomposites, preventing α-helical ordering, but promoting inter-molecular hydrogen bonded β-sheet formation. Depending on peptide and CNC content, the Young's modulus varies from 10 to 150 MPa. Unlike conventional cellulose-reinforced polymer nanocomposites, the mechanical properties of these composite materials are dictated by a balance of CNC reinforcement, peptidic ordering, and microphase-separated morphology. This research highlights that leveraging peptide–cellulose interactions is a strategy to create materials with targeted mechanical properties for a specific application using a limited selection of building blocks.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Material extrusion additive manufacturing of wood pulp-reinforced epoxy composites

Direct ink writing (DIW) is an extrusion-based form of 3D-printing that has gained popularity over the last decade. DIW uses thixotropic fluid extrusion to form a particular shape. In order to form stable structures, the rheology of the paste is important to allow for extrusion from the syringe, stability of the growing print, and prevention of unwanted seeping flow during jog moves. In this work, we use wood pulp as a bio-based filler that can provide shear thinning properties to the ink, which produces a stable ink for DIW processing. Additionally, the filler imparts improved mechanical and thermal performance compared to neat resin. The wood pulp provided the shear thinning behavior necessary for DIW printing, and pulp loadings greater than 6 wt%, provided sufficient yield stress so that the composite could self-support during printing. Nanoclay was utilized to further improve ink rheology and appearance to enable larger scale printing. Overall, this work showed successful DIW of an epoxy resin with a sustainable filler improving its stiffness and thermal properties and provides an avenue for further development of bio-based inks for DIW towards various applications.

Lamm, Meghan E. [Oak Ridge National Laboratory (OR↗

DOE OSTI2025

Harnessing peptide–cellulose interactions to tailor the performance of self-assembled, injectable hydrogels

Taking inspiration from natural systems, such as spider silk and mollusk nacre, that employ hierarchical assembly to attain robust material performance, we leveraged matrix–filler interactions within reinforced polymer–peptide hybrids to create self-assembled hydrogels with enhanced properties. Specifically, cellulose nanocrystals (CNCs) were incorporated into peptide–polyurea (PPU) hybrid matrices to tailor key hydrogel features through matrix–filler interactions. Herein, we examined the impact of peptide repeat length and CNC loading on hydrogelation, morphology, mechanics, and thermal behavior of PPU/CNC composite hydrogels. The addition of CNCs into PPU hydrogels resulted in increased gel stiffness; however, the extent of reinforcement of the nanocomposite gels upon nanofiller inclusion also was driven by PPU architecture. Temperature-promoted stiffening transitions observed in nanocomposite PPU hydrogels were dictated by peptide segment length. Analysis of the peptide secondary structure confirmed shifts in the conformation of peptidic domains (α-helices or β-sheets) upon CNC loading. Finally, PPU/CNC hydrogels were probed for their injectability characteristics, demonstrating that nanofiller–matrix interactions were shown to aid rapid network reformation (∼10 s) upon cessation of high shear forces. Overall, this research showcases the potential of modulating matrix–filler interactions within PPU/CNC hydrogels through strategic system design, enabling the tuning of functional hydrogel characteristics for diverse applications.

42 ENGINEERING↗

DOE OSTI2022

Thermal conductivity of multilayer polymer-nanocomposite thin films

The development of electrical insulators that are thermally conducting is critical for thermal management applications in many advanced electronics and electrical devices. Here, we synthesized polymer nanocomposite (PNC) films composed of polymers [polyethylenimine, poly(vinylamine), poly(acrylic acid), and poly(ethylene oxide)] and dielectric fillers (montmorillonite clay and hexagonal boron nitride) by layer-by-layer technique. The cross-plane thermal conductivity (k⊥) of the film was measured by the 3ω method. The effect of various factors such as film growth, filler type, filler volume fraction, polymer chemical structures, and temperature on the thermal conductivity is reported. The k⊥ of PNCs with thickness from 37 nm to 1.34 μm was found to be in the range of 0.11 to 0.21 ± 0.02 W m−1 K−1. The k⊥ values were found to be lower than the constituent polymer matrix. The experimental result is compared with existing theoretical models of nanocomposite systems to get insight into heat transfer behavior in such layered films composed of dielectrics and polymers.

Physics↗

DOE OSTI2020

Tritium Effects on Aromatic Carbon–Loaded Polymers

By incorporating carbon nanotubes (CNTs) and graphene nanomaterials with aromatic sp2 carbon structures, we have specifically tuned filled ethylene propylene diene monomer elastomer (EPDM) seal and gasket composite materials for radiation resistance. Our results show that CNTs and graphene have an increased ability to stabilize the EPDM matrix compared to standard carbon black (CB) as a radiation-resistant filler. Here, graphene outperforms both CNT and CB fillers when considering surface damage under conditions where beta exposure is an issue. Both graphene and CNT fillers offer significantly reduced changes in glass transition temperature under prolonged exposure to tritium compared to CB-filled standards, with a 2.5-fold and almost 5-fold reduction, respectively. Thus, CNT- and graphene-filled O-ring materials could be designed that would maintain acceptable seals significantly longer than currently used composites.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2023

Effect of fiber reinforcement on the process parameters of injection molding manufacturing process

Use of fillers with the resin is common in injection molding manufacturing technique to enhance the stiffness and strength of the manufactured components. However, the addition of fillers changes the rheological and mechanical properties of the material, required adjustments in the process parameters used for the manufacturing. The present study aims to investigate this impact of fillers on the process parameters of the injection molding manufacturing process. Neat Acrylonitrile Butadiene Styrene (ABS) and ABS reinforced with short glass fibers are used as the materials to perform the comprehensive numerical analysis including complete process sequence, namely filling, packing, cooling and warpage. Parametric studies are conducted to optimize the manufacturing process for minimal warpage (or shrinkage) in the produced part. The selected process parameters for the parametric study include cooling time, packing pressure, and mold temperature, all of which directly impact the quality of the manufactured parts. The optimal values obtained for these parameters are compared to examine the effect fiber reinforcement has on the manufacturing process.

Garg, Nikhil↗

DOE OSTI2023

High Strength, Encapsulated, Commercially Useful Components and Particles Made from Coal Combustion Residuals

This project has developed and demonstrated two high-volume applications for Coal Combustion Residuals (CCR) with annual usage on the order of billions of pounds. The CCR is encapsulated in a recently developed water-impervious inorganic resin coating to reduce leaching of toxic elements from CCR by more than 80% as a first step. Target commercial applications demonstrated for the encapsulated CCR were as reinforcement for high-strength structural columns composed of CCR embedded in a ceramic matrix and as filler in high-volume plastics such as polypropylene. The encapsulated particles produced columns with properties superior to concrete, and a 30% to 50% improvement in stiffness over current fillers in plastics. CCR from bituminous and lignite coal was evaluated and shown to provide high performance, with the bituminous CCR producing the strongest columns and the lignite-based CCR provided the best performance as coated filler in polypropylene. The two-year project advanced both material systems from a Technology Readiness Level (TRL) of 2 to TRL 4.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2021

Tuning Thermal and Mechanical Properties of Polydimethylsiloxane with Carbon Fibers

In order to meet the needs of constantly advancing technologies, fabricating materials with improved properties and predictable behavior has become vital. To that end, we have prepared polydimethylsiloxane (PDMS) polymer samples filled with carbon nanofibers (CFs) at 0, 0.5, 1.0, 2.0, and 4.0 CF loadings (w/w) to investigate and optimize the amount of filler needed for fabrication with improved mechanical properties. Samples were prepared using easy, cost-efficient mechanical mixing to combine the PDMS and CF filler and were then characterized by chemical (FTIR), mechanical (hardness and tension), and physical (swelling, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and coefficient of thermal expansion) analyses to determine the material properties. We found that hardness and thermal stability increased predictably, while the ultimate strength and toughness both decreased. Repeated tension caused the CF-filled PDMS samples to lose significant toughness with increasing CF loadings. The hardness and thermal degradation temperature with 4 wt.% CF loading in PDMS increased more than 40% and 25 °C, respectively, compared with the pristine PDMS sample. Additionally, dilatometer measurements showed a 20% decrease in the coefficient of thermal expansion (CTE) with a small amount of CF filler in PDMS. In this study, we were able to show the mechanical and thermal properties of PDMS can be tuned with good confidence using CFs.

degradation temperature↗

NASA NTRS1972

An intumescent coating for improved fuel fire protection of heat sensitive articles.

Intumescent coating compositions have been prepared using the ammonium salt of 4-nitroaniline-2-sulfonic acid and a copolymer of polysulfide-epoxy resin as the binder, into which have been dispersed various fillers. The fillers used in the study were low density microballoons for density control and fibers for controlled intumescence on contoured substrates. The filler effect on the thermal-physical efficiency of coatings has been measured. The coating utilizing short length silica fibers has been shown to have superior mechanical, environmental, and thermal properties. The coating applied to the exterior of loaded weapons has increased the time-to-detonation from three minutes for the unprotected weapon to 10-13 minutes.

Sawko, P. M.↗

NASA NTRS1977

Intumescent-ablators as improved thermal protection materials

Nitroaromatic amine-based intumescent coatings were improved with regard to their thermal protection ability by adding endothermic decomposing fillers with endotherms at or near the exothermic reaction of the intumescent agent, since the effectiveness of the intumescent coatings without fillers is reduced by the exothermic behavior of the coatings during thermal activation. Fillers were dispersed directly in the base coating. Potassium fluoborate, ammonium fluoborate, zinc borate, and ammonium oxalate function as endothermic ablative materials at specific temperature regions, and also enhance the char formation during the intumescent process.

Sawko, P. M.↗

NASA NTRS1980

Equilibrium swelling of elastomers in solvents

Two proposed empirical equations, developed from Eilers-VanDijk equation to characterize relative modulus of filled elastomers as function of filler content, describe: (1) equilibrium swelling for cases where fillers are composed of permanent aggregates of primary particles; and (2) equilibrium swelling when filler material is composed of non-aggregated particles.

Fedors, R. F.↗

NASA NTRS1980

Recirculating sprayer for fiber-filled paints

Recirculating paint sprayer applies spray of coarse filler in highly volatile solvent. Sprayer was developed for applying insulation material containing epxoy resin, glass fibers, and inert fillers suspended in chlorinated solvents. Sprayer resists abrasive action of fiberglass filler and chemical activity of solvent. Pump and position ensure more uniform pressure at spray gun without backpressure regulator, which tended to clog in old sprayer.

Major, R. K.↗

NASA NTRS1979

Control of volume resistivity in inorganic organic separators

Control of resistivity in NASA inorganic-organic separators is achieved by incorporating small percentages of high surface area, fine particle silica with other ingredients in the separator coating. The volume resistivity is predictable from the surface area of filler particles in the coating. The approach is applied to two polymer- plasticizer -filler coating systems, where the filler content of each is below the generally acknowledged critical pigment volume concentration of the coating. Application of these coating systems to 0.0254 cm thick (10-mil) fuel cell grade asbestos sheet produces inexpensive, flexible, microporous separators that perform as well as the original inorganic-organic concept, the Astropower separator.

Sheibley, D. W.↗

NASA NTRS1980

Control of volume resistivity in inorganic-organic separators

Control of resistivity in NASA inorganic-organic separators is achieved by incorporating small percentages of high surface area, fine-particle silica with other ingredients in the separator coating. The volume resistivity appears to be predictable from coating composition, that is, from the surface area of filler particles in the coating. The approach has been applied to two polymer-'plasticizer'-filler coating systems, where the filler content of each is below the generally acknowledged critical pigment volume concentration of the coating. Application of these coating systems to 0.0254 cm thick (10 mil) fuel-cell grade asbestos sheet produces inexpensive, flexible, microporous separators that perform at least as well as the original inorganic-organic concept, the Astropower separator.

Sheibley, D. W.↗