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At least 433 records · Page 24

Methods of preparing polyimides and artifacts composed thereof

Methods of converting essentially unpolymerized precursors into polyimides in which the precursors are exposed to microwave radiation. Preheating, thermal post-curing, and other techniques may be employed to promote the development of optimum properties; and reinforcements can be employed to impart strength and rigidity to the final product. Also disclosed are processes for making various composite artifacts in which non-polymeric precursors are converted to polyimides by using the techniques described above.

Gagliani, John↗

Methods of preparing polyimides and artifacts composed thereof

Methods of converting essentially unpolymerized precursors into polyimides in which the precursors are exposed to microwave radiation. Preheating, thermal post-curing, and other techniques may be employed to promote the development of optimum properties; and reinforcements can be employed to impart strength and rigidity to the final product. Also disclosed are processes for making various composite artifacts in which non-polymeric precursors are converted to polyimides by using the techniques described above.

Gagliani, John↗

Methods of preparing polyimides and artifacts composed thereof

Methods of converting essentially unpolymerized precursors into polyimides in which the precursors are exposed to microwave radiation. Preheating, thermal post-curing, and other techniques may be employed to promote the development of optimum properties; and reinforcements can be employed to impart strength and rigidity to the final product. Also disclosed are processes for making various composite artifacts in which non-polymeric precursors are converted to polyimides by using the techniques described above.

Gagliani, John↗

Aromatic polyimides containing a dimethylsilane-linked dianhydride

A high-temperature stable, optically transparent, low dielectric aromatic polyimide is prepared by chemically combining equimolar quantities of an aromatic dianhydride reactant and an aromatic diamine reactant, which are selected so that one reactant contains at least one Si(CH.sub.3).sub.2 group in its molecular structure, and the other reactant contains at least one --CH.sub.3 group in its molecular structure. The reactants are chemically combined in a solvent medium to form a solution of a high molecular weight polyamic acid, which is then converted to the corresponding polyimide.

St. Clair, Anne K.↗

Electrically conductive polyimides containing silver trifluoroacetylacetonate

Polyimides with enhanced electrical conductivity are produced by adding a silver ion-containing additive to the polyamic acid resin formed by the condensation of an aromatic dianhydride with an aromatic diamine. After thermal treatment the resulting polyimides had surface conductivities in the range of 1.7.times.10.sup.-3 4.5 .OMEGA..sup.-1 making them useful in low the electronics industry as flexible, electrically conductive polymeric films and coatings.

Rancourt, James D.↗

Tough, processable simultaneous semi-interpenetrating polyimides

A high temperature semi-interpenetrating polymer network (semi-IPN) was developed which had significantly improved processability, damage tolerance and mechanical performance, when compared to the commercial Thermid.RTM. materials. This simultaneous semi-IPN was prepared by mixing a thermosetting polyimide with a thermoplastic monomer precursor solution (NR-15082) and allowing them to react upon heating. This reaction occurs at a rate which decreases the flow and broadens the processing window. Upon heating at a higher temperature, there is an increase in flow. Because of the improved flow properties, broadened processing window and enhanced toughness, high strength polymer matrix composites, adhesives and molded articles can now be prepared from the acetylene endcapped polyimides which were previously inherently brittle and difficult to process.

Pater, Ruth H.↗

Magnetic Property Measurements on Single Wall Carbon Nanotube-Polyimide Composites

Temperature and magnetic field dependent magnetization measurements were performed on polyimide nanocomposite samples, synthesized with various weight percentages of single wall carbon nanotubes. It was found that the magnetization of the composite, normalized to the mass of nanotube material in the sample, decreased with increasing weight percentage of nanotubes. It is possible that the interfacial coupling between the carbon nanotube (CNT) fillers and the polyimide matrix promotes the diamagnetic response from CNTs and reduces the total magnetization of the composite. The coercivity of the samples, believed to originate from the residual magnetic catalyst particles, was enhanced and had a stronger temperature dependence as a result of the composite synthesis. These changes in magnetic properties can form the basis of a new approach to investigate the interfacial properties in the CNT nanocomposites through magnetic property measurements.

Sun, Keun J.↗

Polyimide Resins Resist Extreme Temperatures

Spacecraft and aerospace engines share a common threat: high temperature. The temperatures experienced during atmospheric reentry can reach over 2,000 F, and the temperatures in rocket engines can reach well over 5,000 F. To combat the high temperatures in aerospace applications, Dr. Ruth Pater of Langley Research Center developed RP-46, a polyimide resin capable of withstanding the most brutal temperatures. The composite material can push the service temperature to the limits of organic materials. Designed as an environmentally friendly alternative to other high-temperature resins, the RP-46 polyimide resin system was awarded a 1992 "R&D 100" award, named a "2001 NASA Technology of the Year," and later, due to its success as a spinoff technology, "2004 NASA Commercial Invention of the Year." The technology s commercial success also led to its winning the Langley s "Paul F. Holloway Technology Transfer Award" as well as "Richard T. Whitcom Aerospace Technology Transfer Award" both for 2004. RP-46 is relatively inexpensive and it can be readily processed for use as an adhesive, composite, resin molding, coating, foam, or film. Its composite materials can be used in temperatures ranging from minus 150 F to 2,300 F. No other organic materials are known to be capable of such wide range and extreme high-temperature applications. In addition to answering the call for environmentally conscious high-temperature materials, RP-46 provides a slew of additional advantages: It is extremely lightweight (less than half the weight of aluminum), chemical and moisture resistant, strong, and flexible. Pater also developed a similar technology, RP-50, using many of the same methods she used with RP-46, and very similar in composition to RP-46 in terms of its thermal capacity and chemical construction, but it has different applications, as this material is a coating as opposed to a buildable composite. A NASA license for use of this material outside of the Space Agency as well as additional government-funded testing proved that RP-46 is even more exceptional than originally thought.

Source record↗

Fabrication of Polyimide-Matrix/Carbon and Boron-Fiber Tape

The term HYCARB denotes a hybrid composite of polyimide matrices reinforced with carbon and boron fibers. HYCARB and an improved process for fabricating dry HYCARB tapes have been invented in a continuing effort to develop lightweight, strong composite materials for aerospace vehicles. Like other composite tapes in this line of development, HYCARB tapes are intended to be used to build up laminated structures having possibly complex shapes by means of automated tow placement (ATP) - a process in which a computer-controlled multiaxis machine lays down prepreg tape or tows. The special significance of the present process for making dry HYCARB for ATP is that it contributes to the reduction of the overall cost of manufacturing boron-reinforced composite-material structures while making it possible to realize increased compression strengths. The present process for making HYCARB tapes incorporates a "wet to dry" process developed previously at Langley Research Center. In the "wet to dry" process, a flattened bundle of carbon fiber tows, pulled along a continuous production line between pairs of rollers, is impregnated with a solution of a poly(amide acid) in N-methyl-2-pyrrolidinone (NMP), then most of the NMP is removed by evaporation in hot air. In the present case, the polyamide acid is, more specifically, that of LaRC. IAX (or equivalent) thermoplastic polyimide, and the fibers are, more specifically, Manganite IM7 (or equivalent) polyacrylonitrile- based carbon filaments that have a diameter of 5.2 m and are supplied in 12,000-filament tows. The present process stands in contrast to a prior process in which HYCARB tape was made by pressing boron fibers into the face of a wet carbon-fiber/ poly(amide acid) prepreg tape . that is, a prepreg tape from which the NMP solvent had not been removed. In the present process, one or more layer(s) of side-by-side boron fibers are pressed between dry prepreg tapes that have been prepared by the aforementioned gwet to dry h process. The multilayer tape is then heated to imidize the matrix material and remove most of the remaining solvent, and is pressed to consolidate the multiple layers into a dense tape. For tests, specimens of HYCARB tapes and laminated composite panels made from HYCARB tape were prepared as follows: HYCARB tapes were fabricated as described above. Each panel was made by laying down ten layers of tape, containing, variously, one, two, or three boron-fiber plies and the remainder carbon- fiber-only plies (see figure). Each panel was made by laying down ten layers of tape. Each panel was then cured by heating to a temperature of 225 C for 15 minutes, then pressing at 200 psi (A1.4 MPa) while heating to 371 C, holding at 371 C for 1 hour, then continuing to hold pressure during cooling. Control specimens that were otherwise identical except that they did not contain boron fibers also were prepared. In room-temperature flexural tests, the HYCARB specimens performed comparably to the control specimens; in room-temperature, open-hole compression tests, the HYCARB specimens performed slightly better, by amounts that increased with boron content.

Belvin, Harry L.↗

Stable Polyimides for Terrestrial and Space Uses

Polyimides of a recently developed type have an attractive combination of properties, including low solar absorptivity (manifested as low color) when cast into thin films, resistance to atomic oxygen and ultraviolet radiation, solubility in organic solvents, high glass-transition temperatures, and high thermal stability. The focus of the development work was on polymers that can endure the space environment and that have specific combinations of properties for use on Gossamer spacecraft. Because of their unique combination of properties, these polymers are also expected to find use in a variety of other applications on Earth as well as in space. Examples of other space applications include membranes on antennas, second-surface mirrors, thermal optical coatings, and multilayer thermal insulation. For both terrestrial and space applications, these polyimides can be processed into various forms, including films, fibers, foams, threads, adhesives, and coatings.

Connell, John W.↗

Out of the Autoclave Fabrication of LaRC[TradeMark] PETI-9 Polyimide Laminates

The NASA Langley Research Center developed polyimide system, LaRC PETI-9, has successfully been processed into composites by high temperature vacuum assisted resin transfer molding (HT-VARTM). To extend the application of this high use temperature material to other out-of-autoclave (OOA) processing techniques, the fabrication of PETI- 9 laminates was evaluated using only a vacuum bag and oven cure. A LaRC PETI-9 polyimide solution in NMP was prepared and successfully utilized to fabricate unidirectional IM7 carbon fiber prepreg that was subsequently processed into composites with a vacuum bag and oven cure OOA process. Composite panels of good quality were successfully fabricated and mechanically tested. Processing characteristics, composite panel quality and mechanical properties are presented in this work. The resultant properties are compared to previously developed LaRC material systems processed by both autoclave and OOA techniques including the well characterized, autoclave processed LaRC PETI-5.

Cano, Robert J.↗

Branched Rod-Coil Polyimide-Poly(Alkylene Oxide) Copolymers and Electrolyte Compositions

Crosslinked polyimide-poly(alkylene oxide) copolymers capable of holding large volumes of liquid while maintaining good dimensional stability. Copolymers are derived at ambient temperatures from amine endcapped amic-acid oligomers subsequently imidized in solution at increased temperatures, followed by reaction with trifunctional compounds in the presence of various additives. Films of these copolymers hold over four times their weight at room temperature of liquids such as ionic liquids (RTIL) and/or carbonate solvents. These rod-coil polyimide copolymers are used to prepare polymeric electrolytes by adding to the copolymers various amounts of compounds such as ionic liquids (RTIL), lithium trifluoromethane-sulfonimide (LiTFSi) or other lithium salts, and alumina.

Meador, Maryann B.↗

Porous Cross-Linked Polyimide-Urea Networks

Porous cross-linked polyimide-urea networks are provided. The networks comprise a subunit comprising two anhydride end-capped polyamic acid oligomers in direct connection via a urea linkage. The oligomers (a) each comprise a repeating unit of a dianhydride and a diamine and a terminal anhydride group and (b) are formulated with 2 to 15 of the repeating units. The subunit was formed by reaction of the diamine and a diisocyanate to form a diamine-urea linkage-diamine group, followed by reaction of the diamine-urea linkage-diamine group with the dianhydride and the diamine to form the subunit. The subunit has been cross-linked via a cross-linking agent, comprising three or more amine groups, at a balanced stoichiometry of the amine groups to the terminal anhydride groups. The subunit has been chemically imidized to yield the porous cross-linked polyimide-urea network. Also provided are wet gels, aerogels, and thin films comprising the networks, and methods of making the networks.

Meador, Mary Ann B.↗

Polyimide Aerogels with Three-Dimensional Cross-Linked Structure

A method for creating a three dimensional cross-linked polyimide structure includes dissolving a diamine, a dianhydride, and a triamine in a solvent, imidizing a polyamic acid gel by heating the gel, extracting the gel in a second solvent, supercritically drying the gel, and removing the solvent to create a polyimide aerogel.

Meador, Mary Ann B.↗

The 3D Printing of Polyimide Aerogels

Polyimide aerogels are a nanoporous material made by extracting the liquid portion of a wet gel and replacing it with air, while still maintaining the porous solid internal architecture. This results in a material with extremely low densities, low thermal conductivities, high internal surfaces areas, and low dielectric constants. Currently, complex aerogel forms are not possible, since they require molds in order to be shaped. To overcome this challenge, we are attempting to use various additive manufacturing techniques to produce complex architectures. Three different approaches are being studied to accomplish this. One is to print using a viscous wet gel and have the structure solidify at the end of the print, another is to use a mixing tip, where a less viscous gel and the final chemical that causes gelation will be mixed as it is printing, allowing it to gel layer by layer, and the third is to use a UV curable aerogel with a UV light following behind to solidify the gel as it prints. To have these approaches be successful, the printing parameters and the aerogel's chemical formulation need to be optimized. The more harmonious these two factors can be made, the more defined and complex the resulting structure can be. Preliminary results show that 3D printing polyimide aerogels are a viable option, but further optimization must occur for reliable printing.

Nosel, Theresa↗

Key Features of Polyimide-Derived Carbon Molecular Sieves

Carbon molecular sieve (CMS) membranes have impressive separation properties; however, both chemical and morphology structures need to be understood better. Here we characterize CMS with the simplest polyimide (PI) PMDA/pPDA (PMDA=pyromellitic dianhydride, pPDA=p-phenylenediamine), using FTIR, solid-state 15 N-NMR and 13 C-NMR, XPS, XRD, and Raman spectra to study chemical structure. Here we also compare gas separation properties for this CMS to a CMS derived from a more conventional PI precursor. The detailed characterization shows the presence of aromatic pyridinic, pyrrolic rings as well as graphitic, pyridonic components and a few other groups in both CMS types derived from the very different precursors. The CMS morphologies, while related to precursor and pyrolysis temperature details, show similarities consistent with a physical picture comprising distributed molecular sieving plate-like structures. These results assist in understanding diverse CMS membrane separation performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Polyimide as a durable cathode for all-solid-state Li(Na)–organic batteries with boosted cell-level energy density

The integration of organic electrode materials (OEMs) with solid-state electrolytes (SSEs) is expected to build an all-solid-state battery (ASSB) with long-term sustainability, high safety, and high energy density. Despite this great promise, the cell-level energy density is still far from practically applicable, which stems from the ultrathick SSE layer and thin cathode layer used in a pellet-type ASSB design. Here, a cost-effective polyimide (PI) material was first exploited as an organic cathode for sulfide-based ASSBs. A capacity of ~190 mAh g -1 was delivered with almost no capacity decay over 300 cycles. Moreover, for the first time, a dry-film approach was introduced to manufacture a sheet-type Li–organic ASSB with an ultrathin SSE layer and a high-areal-loading PI cathode. Notably, PI is a perfect candidate for dry-film technology due to its high thermal stability and extraordinary chemical inertness toward sulfide SSEs. Remarkably, the free-standing SSE membrane was merely 46 μm thick, and an ultralow areal resistance of 3.3 Ω cm 2 was achieved, more than tenfold lower than that of reported SSE pellets. One order of magnitude boost in the cell-level energy density was achieved. This work presents a significant leap in transferring organic ASSB technology from laboratory research to factory manufacturing.

25 ENERGY STORAGE↗

Hygrothermal aging effects on polyimide and acrylate-based adhesive materials in high-performance flat-flex cable assemblies

Flat-flex assemblies are widely used across a diverse range of technologies, including consumer electronics, automotive systems, aerospace and defense applications, and medical devices, due to their compact form factor and flexibility. However, environmental stressors like temperature and humidity are known to degrade performance over time, though the main mechanisms for degradation remain unknown. Here, in this work, we examined the aging behavior of copper/polyimide/adhesive laminate systems under varying temperature and humidity conditions, focusing on material degradation and its effects on mechanical and dielectric properties. Results show that peel strength and breakdown voltage decrease with exposure time, temperature, and humidity; spectroscopic characterization revealed that the adhesive, and not the polyimide, is the weak link in the material stack-up. The adhesive, identified as a butyl acrylate-acrylonitrile (BA-AN) copolymer, exhibited age-related spectral changes that correlated with exposure severity and duration. Hydrolysis at BA ester and AN nitrile groups was identified as the primary degradation mechanism, producing amides, acids, and alcohols. We developed a mechanistic model that connects kinetic parameters for BA-AN spectral band decay to peel strength and breakdown voltage, and implicates hydrolysis at the AN moiety, not BA, in performance decrements. Modeling predictions at ambient conditions indicate faster decline in peel strength than dielectric strength at early times, followed by plateauing of both properties at longer times. These findings provide critical insights into laminate aging mechanisms and highlight the importance of addressing BA-AN degradation to improve the long-term reliability of these systems in high-humidity environments.

organic↗