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At least 271 records · Page 15
All sourcesNASA NTRSDOE OSTI
NASA NTRS2015

Polyimides Derived from Novel Asymmetric Benzophenone Dianhydrides

This invention relates to the composition and processes for preparing thermoset polyimides derived from an asymmetric dianhydride, namely 2,3,3',4'-benzophenone dianhydride (a-BTDA) with at least one diamine, and a monofunctional terminal endcaps. The monofunctional terminating groups include 4-phenylethynylphthalic anhydride ester-acid derivatives, phenylethyl trimellitic anhydride (PETA) and its ester derivatives as well as 3-phenylethynylaniline. The process of polyimide composite comprises impregnating monomer reactants of dianhydride or its ester-acid derivatives, diamine and with monofunctional reactive endcaps into glass, carbon, quartz or synthetic fibers and fabrics, and then stack up into laminates and subsequently heated to between 150-375.degree. C. either at atmosphere or under pressure to promote the curing and crosslinking of the reactive endcaps to form a network of thermoset polyimides.

Chuang, Chun-Hua↗
NASA NTRS2020

Ionic Polyimides: New High Performance Polymers for Additive Manufacturing

There is currently a very limited set of engineering polymers that have been demonstrated as viable for use in 3-D printing. Additive manufacturing of custom components will require a much larger array of polymers, especially those with physical, thermal, chemical, and mechanical properties that can be tailor-made. The development of ‘Ionic Polyimides’ offers a solution to this shortage by combining the well understood and widely accepted properties of conventional polyimides, with a new approach to polymer synthesis. Polyimides and polymeric ionic liquids (poly(ILs)) are at the forefront of advanced polymer materials, each with their own set of advantages and disadvantages. While it is clear that more types of polymer materials are needed for fused deposition modeling (FDM) additive manufacturing, there is a need to explore these classes of materials. The synthesis process developed by the Bara Research Group at the University of Alabama allows full control over polymer structure, nanostructure, thermal, electrical, and physical properties making them a prime candidate for use in the additive manufacturing process.

Jackson, Enrique↗
DOE OSTI2020

Free volume manipulation of a 6FDA-HAB polyimide using a solid-state protection/deprotection strategy

We report tert-butoxycarbonyl (t-BOC) is a thermally labile moiety that can be used to protect hydroxyl groups on polymers. In this study, t-BOC was appended onto a polyimide consisting of 2,2'-bis-(3,4-dicarboxyphenyl) hexafluoropropane dianhydride (6FDA) and 3,3'-dihydroxy-4,4'-diamino-biphenyl (HAB), after which the polymer was formed into self-standing films. Solid-state thermal treatments were performed to systematically remove t-BOC moieties to alter the physical packing structure and concomitant gas transport properties of the polymer. Despite performing deprotection reactions well below the glass transition temperature of 6FDA-HAB (~300 °C), this free volume manipulation (FVM) approach produced only subtle differences in polymer density, fractional free volume, average free volume element size, and gas transport properties relative to the unprotected polymer. While these findings suggest that thermally removing covalently bound functional groups from polymer films can be used to manipulate free volume and gas transport performance for glassy polymers, more robust polymer systems than linear polyimides are required to preserve the nascent free volume architecture generated from this approach.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Tuning gas separation performance of polyimide membranes with macrocyclic crown ether units

Membrane-based gas separation is an energy-efficient alternative to conventional thermally-driven separation processes. However, polymer membranes face the permeability-selectivity trade-off challenge, which stems from the broad size distribution of free volume voids. Here, this study reports a molecular design strategy to address this challenge through incorporating macrocyclic crown ether (CE) moieties into the backbone of Matrimid® polyimide, a commercial gas separation membrane. A series of CE-containing Matrimid®-like copolyimides were synthesized with systematically varied CE molar contents ranging from 3 to 20%. These copolyimides formed ductile, defect-free thin films suitable for membrane fabrication. Gas permeation tests revealed a non-monotonic relationship between permeability/selectivity and CE content. Notably, the copolyimide with only 5% CE demonstrated a 61% increase in CO 2 /CH 4 selectivity and a 13% increase in CO 2 permeability relative to pristine Matrimid®. Higher CE contents did not yield further performance improvements, which is likely due to the competing effects of chain packing disruption and π–π interactions among CE moieties at high content. This hypothesis was supported by wide-angle X-ray scattering (WAXS) analysis, density measurements, and fractional free volume calculations. These findings highlight the potential of macrocyclic crown ether incorporation strategies in fine tuning the microstructure of commercial polyimide gas separation membranes to surpass the traditional permeability-selectivity trade-off.

CO2 separation↗
NASA NTRS2013

Slotted Polyimide-Aerogel-Filled-Waveguide Arrays

This presentation discussed the potential advantages of developing Slotted Waveguide Arrays using polyimide aerogels. Polyimide (PI) aerogels offer great promise as an enabling technology for lightweight aerospace antenna systems. PI aerogels are highly porous solids possessing low density and low dielectric permittivity combined with good mechanical properties. For slotted waveguide array applications, there are significant advantages in mass that more than compensate for the slightly higher loss of the aerogel filled waveguide when compared to state of practice commercial waveguide.

Slotted Waveguide Arrays↗
NASA NTRS2017

Novel Polyimide Battery Separator Imbibed with Room-Temperature Ionic Liquids

The journey to Mars will require advancements in many existing technologies, including space power and energy storage systems. According to the 2015 NASA Technology Roadmaps, energy storage is a critical technology area to develop for both terrestrial as well as future long-term space missions. Currently, batteries represent one of the major areas in need of advancement, both in terms of energy density as well as safety. Recently, concerns regarding the fire safety of commercial lithium-ion batteries have prompted efforts to produce nonflammable battery components, namely the electrolyte and separator. Commercial lithium-ion batteries utilize polyolefin separators imbibed with a lithium salt dissolved in cyclic carbonates. This separator/electrolyte combination imparts good ionic conductivities in the range of 10(exp -2) to 10(exp -3) S/cm. However, the cyclic carbonates and polyolefin separator are inherently flammable. Room-temperature ionic liquids (RTILs) appear to be a safer alternative to cyclic carbonates. They offer good ionic conductivities, similar to those observed in cyclic carbonates, but are inherently nonvolatile and nonflammable giving them a safety advantage. Many promising RTILs for battery electrolytes are not compatible with commercial polyolefin separator materials. Polyimide aerogels possess an open-porous, fibrillar network architecture which offers a high degree of porosity (typically greater than 85 porous), required for lithium ion conduction, as well as good mechanical properties. Furthermore, these materials are compatible with all tested RTILs. By creating a polyimide gel and imbibing the gel with a RTIL containing a lithium salt instead of super critically drying them to form aerogels, a nonflammable separator/electrolyte system with conductivities in the range of 1x10(exp -3) S/cm has been demonstrated.

Polyimide↗
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 OSTI2022

Polyimide aerogels for ballistic impact protection

The ballistic performance of edge-clamped monolithic polyimide aerogel blocks (12 mm thickness) has been studied through a series of impact tests using a helium-filled gas gun connected to a vacuum chamber and a spherical steel projectile (approximately 3 mm diameter) with an impact velocity range of 150–1300 m s -1 . The aerogels had an average bulk density of 0.17 g cm -3 with high porosity of approximately 88%. The ballistic limit velocity of the aerogels was estimated to be in the range of 175–179 m s -1 . Moreover, the aerogels showed a robust ballistic energy absorption performance (e.g., at the impact velocity of 1283 m s -1 at least 18% of the impact energy was absorbed). At low impact velocities, the aerogels failed by ductile hole enlargement followed by a tensile failure. By contrast, at high impact velocities, the aerogels failed through an adiabatic shearing process. Given the substantially robust ballistic performance, the polyimide aerogels have a potential to combat multiple constraints such as cost, weight, and volume restrictions in aeronautical and aerospace applications with high blast resistance and ballistic performance requirements such as in stuffed Whipple shields for orbital debris containment application.

42 ENGINEERING↗
DOE OSTI2024

Mechanical and electrical changes in electrochemically active polyimide binders for Li-ion batteries

Polyimide binders are often used in electrodes made with silicon for lithium-ion batteries for their mechanical strength and adhesion, which help mitigate mechanical issues associated with large volumetric expansion. These binders can be electrochemically active, but it is difficult to characterize what physical and chemical changes occur due to a composite electrode with multiple components and processes at play. Here, in this work, we study electrodes consisting only of polyimide binder and conductive carbon, using scanning probe-based techniques—contact resonance, force volume, and scanning spreading resistance microscopy—along with cryo-scanning transmission electron microscopy, electron energy loss spectroscopy, and energy dispersive X-ray spectroscopy. We show that lithium becomes trapped in the binder during cycling and results in large initial capacity losses, the formation of dendrite-like features, column-like domains of significantly increased mechanical modulus, and a slight increase in electronic resistivity.

25 ENERGY STORAGE↗
NASA NTRS1970

Soluble high molecular weight polyimide resins

High molecular weight polyimide resins have greater than 20 percent /by weight/ solubility in polar organic solvents. They permit fabrication into films, fibers, coatings, reinforced composite, and adhesive product forms. Characterization properties for one typical polyimide resin are given.

Jones, R. J.↗
NASA NTRS1972

Polyimide foams provide thermal insulation and fire protection

Chemical reactions to produce polyimide foams for application as thermal insulation and fire prevention materials are discussed. Thermal and physical properties of the polyimides are described. Methods for improving basic formulations to produce desired qualitites are included.

Rosser, R. W.↗
NASA NTRS1971

Development of a low void polyimide resin for autoclave processing of glass and graphite reinforced composites.

Experimental studies are described in which new A-type polyimide prepolymer chemical modifications were investigated with the aim of increasing the melt phase duration and temperature range permitting autoclave processing, yet retaining the addition-type cure mechanism required for low-void content composites. Several modification candidates were examined, and one specific formulation was selected for detailed investigation. This A-type polyimide prepolymer formulation is shown to possess the desired characteristics.

Vaughan, R. W.↗
NASA NTRS1973

Preparation of polyimides from mixtures of monomeric diamines and esters of polycarboxylic acids

Polyimides having high thermal and oxidative stability are prepared by the reaction of a mixture of monomers comprising (1) a dialkyl or tetraalkyl ester of an aromatic tetracarboxylic acid; (2) an aromatic diamine; and (3) a monoalkyl or dialkyl ester of a dicarboxylic acid where in the ratio of a:b:c is n:(n+1):2, wherein n has a value from 1 to 20. The mixture of monomers is prepared in a 30 to 70 percent by weight solution of an organic solvent, a substrate impregnated with the solution and heated at 50 to 205 C to remove said solvent and form a low molecular weight prepolymer, and thereafter heated at 275 to 350 C to cure to a high molecular weight polyimide.

Serafini, T. T.↗
NASA NTRS1972

Development and evaluation of graphite and boron polyimide composites.

This paper covers the development and evaluation of the HT-S/710 graphite/polyimide system and initial evaluations of high modulus graphite and boron reinforced polyimide systems. Detail design properties of the HT-S/710 graphite/polyimide systems, test results of test sheet stringer components, and initial test evaluations of high modulus graphite and boron reinforced polyimide composites are presented. Preliminary design applications utilizing the basic processing and design data from this development program are presented as to their utilization in aircraft and space applications.

Scheck, W. G.↗
NASA NTRS1973

Polyimide foam for the thermal insulation and fire protection

The preparation of chemically resistant and flame retardant foams from polyfunctional aromatic carboxylic acid derivatives and organic polyisocyanates is outlined. It was found that polyimide foams of reproducible density above 1 lb./ft. and below 6 lbs./cu ft. can be obtained by employing in the reaction of least 2% by weight of siloxane-glycol copolymer as a surfactant which acts as a specific density control agent. Polyimide foams into which reinforcing fibers such as silicon dioxide and carbon fibers may be incorporated were also produced.

Rosser, R. W.↗
NASA NTRS1975

Dynamic load capacities of graphite fiber: Polyimide composites in oscillating plain bearings to 340 C (650 F)

Load capacities were determined for plain spherical bearings with self-lubricating spherical elements of graphite-fiber-reinforced-polyimide, and for plain cylindrical bearings with thin-wall liners of the composite in the bearing bores. Composites consisted of a 1-to-1 weight ratio of graphite fibers and polyimide. Oscillation was at an amplitude of + or - 15 deg at a frequency of 1 hertz. Bearings with composite ball material had a load capacity of approximately 69 MN/sq m (10 000 psi) at room temperature 25 MN/sq m (3600 psi) at 340 C (650 F). Bearings with thin-wall composite liners had much higher load capacities of 280 MN/sq m (40 000 psi) at room temperature amd 240 MN/sq m (35 000 psi) at 320 C (600 F). Friction coefficients were in the range of 0.12 to 0.19. The addition of 10 wt.% graphite fluoride solid lubricant to the composition of the thin-wall liners reduced friction coefficients into the range of 0.10 to 0.12.

Sliney, H. E.↗
NASA NTRS1975

Isomer effects on polyimide properties

The effect of structure variation on the solubility and glass-transition temperature of polyimide polymers is investigated. The addition of alkyl substituents to an aromatic ring in the polymer molecule, the reduction in the number of imide rings per average polymer chain-length, and a variation in the symmetry of the polymer molecule are studied. The synthesis of key intermediates for the preparation of the monomers required in this investigation is reported along with progress made in the synthesis of polyimide-precursor amines that contain functional groups to allow for post-cure cross-linking.

Stump, B. L.↗