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DOE OSTI2023

Chemically recyclable polyolefin-like multiblock polymers

Polyolefins are the most important and largest volume plastics produced. Unfortunately, the enormous use of plastics and lack of effective disposal or recycling options have created a plastic waste catastrophe. Here in this work, we report an approach to create chemically recyclable polyolefin-like materials with diverse mechanical properties through the construction of multiblock polymers from hard and soft oligomeric building blocks synthesized with ruthenium-mediated ring-opening metathesis polymerization of cyclooctenes. The multiblock polymers exhibit broad mechanical properties, spanning elastomers to plastomers to thermoplastics, while integrating a high melting transition temperature (T m ) and low glass transition temperature (T g ), making them suitable for use across diverse applications (T m as high as 128°C and T g as low as –60°C). After use, the different plastics can be combined and efficiently deconstructed back to the fundamental hard and soft building blocks for separation and repolymerization to realize a closed-loop recycling process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1996

Free Volume in Glassy Poly(arylene Ether Ketone)s

Amorphous polyarylene ether ketones were examined in the glassy state by positron annihilation lifetime spectroscopy ( PALS ) and in the melt by standard rheological techniques. Specimens were well-characterized fractions of two isomeric structures. PALS clearly shows that the polymer with meta linkages in its backbone contains larger voids (greater than 0.25 nm radius). Thus despite their similar bulk densities, the two materials must pack very differently on a local scale. On the other hand, the free volumes inferred from the WLF treatment of melt viscosity data are practically identical in both materials ca. 4% at T(sub g). The comparison between techniques sheds some light on the distribution of free volume.

Hinkley, J. A.↗

NASA NTRS2019

Laser Sintering of Thermoset Polyimide Composites

Selective Laser Sintering (SLS) is an additive manufacturing technique that builds 3D models layer by layer using a laser to selectively melt cross sections in powdered polymeric materials, following sequential slices of the CAD model. SLS generally uses thermoplastic polymeric powders, such as polyamides (i.e. Nylon), and the resultant 3D objects are often weaker in their strength compared to traditionally processed materials, due to the lack of polymer inter-chain connection in the z-direction. Our previous effort showed the challenges of printing a melt-processable RTM370 imide resin powder terminated with reactive 4-phenylethynylphthalic anhydride by LS, due to its inherently low viscosity of these oligomers. This paper presented the first successful 3D printing of high temperature carbon fiber filled thermoset polyimide composites, followed by post cure cycles to promote additional crosslinking for achieving higher temperature (Tg = 370 °C) capability. The processes to build tensile specimens and a component by LS, and the characterization of RTM370 imide resin by DSC and rheology as well as evaluation of the LS printed polyimide composite specimens by SEM and mechanical tests will be discussed.

Polyimide Composites↗

DOE OSTI2024

Tailoring the Properties of Chemically Recyclable Polyethylene‐Like Multiblock Polymers by Modulating the Branch Structure

Abstract Developing plastics that fill the need of polyolefins yet are more easily recyclable is a critical need to address the plastic waste crisis. However, most efforts in this vein have focused on high‐density polyethylene (PE), while many different types of PE exist. To create broadly sustainable PE with modular properties, we present the synthesis, characterization, and demonstration of materials applications for chemically recyclable PE‐like multiblock polymers prepared from distinct hard and soft blocks using ruthenium‐catalyzed dehydrogenative polymerization. By altering the branching pattern within the soft blocks, a series of PE‐like multiblock polymers were synthesized with tunable glass transition temperatures ( T g ) while maintaining consistent high melting temperatures ( T m ). A clear U‐shape trend between T g and mechanical properties was found, showcasing their potential as sustainable materials with tailored properties spanning commercial linear low‐density polyethylene (LLDPE) and low‐density polyethylene (LDPE). These materials offer adjustable adhesive strength to metal and demonstrate chemical recyclability and selective depolymerization in mixed plastic streams, promoting circularity and separation.

Zhao, Yucheng↗

NASA NTRS1989

Polyimides containing carbonyl and ether connecting groups - II

In a study of polyimides containing carbonyl and ether connecting groups between aromatic rings, several new polyimides were prepared and characterized. A few of these polymers were semicrystalline. Glass transition temperatures ranged from 164 to 258 C, and crystalline melt temperatures were observed between 350 and 424 C. The semicrystalline polyimide from the reaction of 3.3',4,4'-benzophenonetetracarboxylic dianhydride and 1,3-bis(4-aminophenoxy-4'-benzoyl)benzene provided transparent orange films with excellent tensile properties, exceptional resistance to solvents and strong base, and high thermooxidative stability. In addition, this polyimide provided excellent adhesive strength for joining titanium (6Al-4V) to titanium.

Hergenrother, P. M.↗

NASA NTRS1991

Polycrystalline SiC fibers from organosilicon polymers

Various organosilicon polymers have been converted into small diameter, fine-grained silicon carbide fibers by melt spinning, crosslinking, and pyrolyzing to greater than 1600 C. The high pyrolysis temperature densifies the fiber and causes CO evolution which removes nearly all oxygen. An additive prevents the loss of strength normally associated with such treatments. Silicon carbide fibres with up to 2.6 GPa (380 ksi) tensile strength, greater than 420 GPa (greater than 60 Msi) elastic modulus, and 3.1-3.2 mg/cu m density have been prepared via this process. Their microstructure consists of greater than 95 wt pct B-SiC crystallites averaging 30-40 nm diameter, with varying amounts of graphitic carbon between the SiC grains. Under inert conditions, the fibers can be thermally aged at least 12 h/1800 C with minimal change in properties.

Lipowitz, Jonathan↗

NASA NTRSDate not supplied

A Review of Extra-Terrestrial Regolith Excavation Concepts and Prototypes

Regolith is present on many extra-terrestrial bodies, and the crushed rock material it is made of contains many of the resources that are enabling for In-Situ Resource Utilization (ISRU). When extracted these resources can be used to provide consumables such as rocket propellant, human life support, working fluids and gases for industrial processes and feedstocks for manufacturing. In addition, the regolith can also be very beneficial for construction purposes as an aggregate which can be used for construction materials and shielding for radiation protection and micrometeorite impact. Binders for regolith concrete may also be made from geopolymers that may be in the regolith. The regolith can be melted and drawn out into glass fibers and used as reinforcements in a metal, polymer, or concrete matrix. In addition, there is tremendous scientific and geological knowledge that can only be obtained by studying samples of the regolith. However, none of these valuable activities can proceed without first acquiring the regolith granular material with some type of excavation device and method. Excavation is in the critical path of many workflows that will make up the capabilities required to establish a human and robotic presence in our solar system. While scientific in-situ sampling of regolith in small quantities has been achieved since the dawn of the space age in the 1960’s, large scale excavation for mining and construction on extra-terrestrial bodies has only been contemplated for many decades in works of scientific fact and also in fictional stories, but serious development and prototyping of excavation technologies for use in reduced gravity space environments was only started in the late 1990’s.This paper will review and document the evolution of extra-terrestrial excavation concepts and prototypes based on the available literature and the personal experience of the author who has been working on regolith excavation technology development since 1998.

ISRU↗

NASA NTRSDate not supplied

A Review of Extra-Terrestrial Regolith Excavation Concepts and Prototypes

Regolith is present on many extra-terrestrial bodies, and the crushed rock material it is made of contains many of the resources that are enabling for In-Situ Resource Utilization (ISRU). When extracted, these resources can be used to provide consumables such as rocket propellant, human life support, working fluids and gases for industrial processes and feedstocks for manufacturing. In addition, the regolith can also be very beneficial for construction purposes as an aggregate which can be used for construction materials and shielding for radiation protection and micrometeorite impact. Binders for regolith concrete may also be made from geopolymers that may be in the regolith. The regolith can be melted and drawn out into glass fibers and used as reinforcements in a metal, polymer, or concrete matrix. In addition, there is tremendous scientific and geological knowledge that can only be obtained by studying samples of the regolith. However, none of these valuable activities can proceed without first acquiring the regolith granular material with some type of excavation device and method. Excavation is in the critical path of many workflows that will make up the capabilities required to establish a human and robotic presence in our solar system. While scientific in-situ sampling of regolith in small quantities has been achieved since the dawn of the space age in the 1960’s, large scale excavation for mining and construction on extra-terrestrial bodies has only been contemplated, for many decades, but serious development and prototyping of excavation technologies for use in reduced gravity space environments was only started in the late 1990’s. This paper will review and document the evolution of extra-terrestrial excavation concepts and prototypes based on the available literature and the personal experience of the author who has been working on regolith excavation technology development since 1998.

Regolith↗

NASA NTRSDate not supplied

A Review of Extra-Terrestrial Regolith Excavation Concepts and Prototype

Regolith is present on many extra-terrestrial bodies, and the crushed rock material it is made of contains many of the resources that are enabling for In-Situ Resource Utilization (ISRU). When extracted, these resources can be used to provide consumables such as rocket propellant, human life support, working fluids and gases for industrial processes and feedstocks for manufacturing. In addition, the regolith can also be very beneficial for construction purposes as an aggregate which can be used for construction materials and shielding for radiation protection and micrometeorite impact. Binders for regolith concrete may also be made from geopolymers that may be in the regolith. The regolith can be melted and drawn out into glass fibers and used as reinforcements in a metal, polymer, or concrete matrix. In addition, there is tremendous scientific and geological knowledge that can only be obtained by studying samples of the regolith. However, none of these valuable activities can proceed without first acquiring the regolith granular material with some type of excavation device and method. Excavation is in the critical path of many workflows that will make up the capabilities required to establish a human and robotic presence in our solar system. While scientific in-situ sampling of regolith in small quantities has been achieved since the dawn of the space age in the 1960’s, large scale excavation for mining and construction on extra-terrestrial bodies has only been contemplated, for many decades, but serious development and prototyping of excavation technologies for use in reduced gravity space environments was only started in the late 1990’s. This paper will review and document the evolution of extra-terrestrial excavation concepts and prototypes based on the available literature and the personal experience of the author who has been working on regolith excavation technology development since 1998.

Regolith↗

DOE OSTI2026

Sequence-Structure–Property Relationships in Short-Chain Polyesters: How Primary Structure Governs Macroscopic Performance

While polymer properties are fundamentally linked to their nanostructure, the influence of monomer sequence remains less understood than stereochemical factors like tacticity. This study examines how sequence distribution affects the thermal behavior and morphology of homo- and copolyesters, specifically comparing polymers derived from constitutionally identical monomers but with varying degrees of sequence regularity depending on monomer structure or polymerization selectivity. Our findings show that increasing sequence defects progressively diminish thermal stability, crystallinity, melting temperatures, and morphological order. As new materials become more compositionally complex, this work underscores the importance of sequence control in the design of advanced polymers for emerging applications.

Bocharova, Vera [Oak Ridge National Laboratory (OR↗

NASA NTRS2006

Thermal Conductivity of Ultem(TradeMark)/Carbon Nanofiller Blends

In an effort to improve polymer thermal conductivity (TC), Ultem(TradeMark) 1000 was compounded with nano-fillers of carbon allotropes. Ultem(TradeMark) 1000 was selected since it is both solution and melt processable. As-received and modified multiwalled carbon nanotubes (MWCNTs), vapor grown carbon nanofibers (CNF) and expanded graphite (EG) were investigated. MWCNTs were modified by functionalizing the surface through oxidization with concentrated acids, mixing with an alkyl bromide, and addition of alkyl and phosphorus compounds after initial treatment with n-butyl lithium. Functionalization was performed to improve the TC compatibility between the resin and MWCNTs. It was postulated that this may provide an improved interface between the MWCNT and the polymer which would result in enhanced TC. The nano-fillers were mixed with Ultem(TradeMark) 1000 in the melt and in solution at concentrations ranging from 5 to 40 wt%. Ribbons were extruded from the blends to form samples where the nano-fillers were aligned to some degree in the extrusion direction. Samples were also fabricated by compression molding resulting in random orientation of the nano-fillers. Thermal properties of the samples were evaluated by Differential Scanning Calorimetry (DSC) and Thermal Gravimetric Analyzer (TGA). Tensile properties of aligned samples were determined at room temperature. The specimens were cut from the ribbons in the extrusion direction; hence the nano-fillers are somewhat aligned in the direction of stress. Typically it was observed that melt mixed samples exhibited superior mechanical properties compared to solution mixed samples. As expected, increased filler loading led to increased modulus and decreased elongation with respect to the neat polymer. The degree of dispersion and alignment of the nano-fillers was determined by high-resolution scanning electron microscopy (HRSEM). HRSEM of the ribbons revealed that the MWCNTs and CNFs were predominantly aligned in the flow direction. The TC of the samples was measured using a Nanoflash(TradeMark) instrument. Since the MWCNTs and CNF are anisotropic, the TC was expected to be different in the longitudinal (parallel to the nanotube and fiber axis) and transverse (perpendicular to the nanotube and fiber axis) directions. The extruded ribbons provided samples for transverse TC measurements. However, to determine the TC in the longitudinal direction, the ribbons needed to be stacked and molded under 1.7 MPa and 270 C. Samples were then obtained by cutting the molded block with a diamond saw. The largest TC improvement was achieved for aligned samples when the measurement was performed in the direction of MWCNT and CNF alignment (i.e. longitudinal axis). Unaligned samples also showed a significant improvement in TC and may be potentially useful in applications when it is not possible to align the nano-filler. The results of this study will be presented.

Ghose, S.↗

DOE OSTI2023

Solid-state polymer magnesium supercapacitor

Here, the present article focuses on the development of a highly ion-conductive, solvent-free, solid-state polymer electrolyte membrane (PEM) via photopolymerization of polyethylene glycol diacrylate (PEGDA) network from its homogeneous melt mixtures containing succinonitrile (SCN) plasticizer and magnesium bis(trifluoromethane sulfonyl) imide Mg(TFSI) 2 salt. The above solid-state Mg-PEM exhibits a Helmholtz electric double-layer capacitor (EDLC) behavior in its supercapacitive symmetric carbonaceous electrode configuration. The electrochemical stability for this PEM membrane (20/40/40 PEGDA/SCN/Mg (TFSI) 2 ) was found to be approximately 3 V from linear sweep voltammetry with a specific capacitance of about 44 F/g from cyclic voltammetry and an energy density of approximately 17 Wh/kg in the 0–2 V range from the constant current density (CCD) experiment. Of particular interest is its excellent capacity retention of over 11,200 cycles, thus tested with the Coulombic efficiency of over 87%. Moreover, the energy density after extensive cycling for 11,200 has increased to approximately 56 Wh/kg at 10 mV/s in the potential range of 0–3 V relative to 17 Wh/kg in the potential range of 0–2 V at the same scan rate, attesting the excellent electrochemical stability and long life of the present Mg-PEM supercapacitor.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS2007

Microgravity Effects on Combustion of Polymers

A viewgraph presentation describing various microgravity effects on the combustion of polymers is shown. The topics include: 1) Major combustion processes and controlling mechanisms in normal and microgravity environments; 2) Review of some buoyancy effects on combustion: melting of thermoplastics; flame strength, geometry and temperature; smoldering combustion; 3) Video comparing polymeric rods burning in normal and microgravity environments; and 4) Relation to spacecraft fire safety of current knowledge of polymers microgravity combustion.

Hirsch, David↗

NASA NTRS1985

Bismaleimides and related maleimido polymers as matrix resins

Significant processing and property improvements can be achieved by copolymerization of state-of-the-art bisimides with various vinyl stilbazole derivatives to give both fire resistance and high-temperature properties from hot-melt compositions. Significant improvement in mechanical properties is achieved through these modifications, which may make these new matrix resins ideal candidates for fireworthy secondary graphite composite structures. Phosphorous modifications of maleimido polymers through phosphonate structure and tricyclophosphazene derivatives provide families of new matrix resins for short-time applications in severe thermo-oxidative environments. With further research these may provide matrix resins for long-term thermo-oxidative stability of advanced composites at temperatures up to 400 to 500 C.

Parker, J. A.↗

NASA NTRS2026

Application of Energy-efficient Electromagnetic Melt-Processing for the Upcycling of Recycled Polyphenylene Sulfide into Multifunctional Segregated Nanocomposites

Polyphenylene sulfide (PPS) is widely used in structural and functional composites because of its thermal stability, chemical resistance, and mechanical strength. As circular manufacturing becomes increasingly important, extending the service life of recycled PPS (rPPS) is essential. However, conventional high-temperature reprocessing accelerates thermo-oxidative degradation, reducing recycled composite performance. This study proposes a rapid and potentially energy-saving upcycling strategy for rPPS using electromagnetic (EM) melt-processing to form segregated carbon nanotube (CNT) networks and produce EM-responsive nanocomposites. The aim was to determine whether CNT-assisted EM heating could reduce polymer degradation while improving multifunctional properties at ultralow filler loadings. rPPS micropellets were coated with CNTs by ball milling to create conductive shells, then compacted into green bodies (GBs) and selectively melted by rapid EM irradiation. Structural, electrical, mechanical, rheological, and electromagnetic interference (EMI) shielding properties were evaluated. Electrical percolation occurred at an ultralow CNT loading of 0.08 wt%, with conductivity reaching (1.24 ± 0.74) × 10 -5 S⋅m -1 at 0.1 wt%. At this concentration, tensile strength and modulus increased by 72% and 99%, respectively. At ~ 0.7 mm thickness, X-band EMI shielding effectiveness reached 6 dB for GBs and 3 dB after EM processing. This shows that EM melt-processing upcycles rPPS into high-performance multifunctional nanocomposites with minimum thermal degradation.

recycled↗

DOE OSTI2023

Shear Assisted Processing and Extrusion (ShAPE) of Plastics: Recycling and Remolding

Polyethylene (PE) and polypropylene (PP) are often disposed as mixed plastic wastes. The challenges in recycling and upcycling these mixed polyolefin wastes lie in the difficulty in separating individual constituents in a cost-effective and scalable manner. Direct recycling the mixed PE and PP wastes in conventional melt-phase extruders typically result in a product with poor properties and low added value, because of immiscibility, phase separation, and lack of crystallinity. Friction extrusion (FE), a solid phase processing technique that has successfully extruded metal matrix composites with desired end products, has never been utilized to address the issue of recycling mixed plastic wastes. In this study, FE was performed on single-stream low-density polyethylene (LDPE), single-stream PP and mixed-stream LDPE+PP. Consolidated filaments of 2.5 mm diameter were extruded from different precursors. The thermal, infrared, and microscopic properties of extruded filaments were measured to evaluate the effects of FE process on the structure of recycled polymers. Meanwhile, the energy efficiency of FE was estimated based on extrusion rates and compared with conventional melt extrusion processes.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2022

Comprehensive view of microscopic interactions between DNA-coated colloids

Abstract The self-assembly of DNA-coated colloids into highly-ordered structures offers great promise for advanced optical materials. However, control of disorder, defects, melting, and crystal growth is hindered by the lack of a microscopic understanding of DNA-mediated colloidal interactions. Here we use total internal reflection microscopy to measure in situ the interaction potential between DNA-coated colloids with nanometer resolution and the macroscopic melting behavior. The range and strength of the interaction are measured and linked to key material design parameters, including DNA sequence, polymer length, grafting density, and complementary fraction. We present a first-principles model that screens and combines existing theories into one coherent framework and quantitatively reproduces our experimental data without fitting parameters over a wide range of DNA ligand designs. Our theory identifies a subtle competition between DNA binding and steric repulsion and accurately predicts adhesion and melting at a molecular level. Combining experimental and theoretical results, our work provides a quantitative and predictive approach for guiding material design with DNA-nanotechnology and can be further extended to a diversity of colloidal and biological systems.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

NASA NTRS1983

Aromatic Polyimides With Group VI Linkages

New polymer system combines thermal and solvent resistant properties of aromatic polyimides with processability of PPX polymers. PPX polymers include polyphenylene oxide, polyphenylene sulfide, and polyphenylene sulfone classes. Generally more processable by hot melt or thermoplastic techniques than aromatic polyimides. PPX systems more susceptible to attack by solvents and have lower glass transition temperatures than PI group.

St. Clair, T. L.↗