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At least 253 records · Page 14

Heat, Moisture and Chemical Resistant Polyimide Compositions and Methods for Making and Using Them

Polyimides having a desired combination of high thermo-oxidative stability, low moisture absorption and excellent chemical and corrosion resistance are prepared by reacting a mixture of compounds including (a) 3,3',4,4'- benzophenonetetracarboxylic dianhydride (BTDA), (b) 3,4'- oxydianiline (3,4'-ODA), and (c) 5-norbornene-2,3- dicarboxylic anhydride (NA) in a high boiling, aprotic solvent to give 5 to 35% by weight of polyamic acid solution. The ratio of (a), (b), and (c) is selected to afford a family of polyimides having different molecular weights and properties. The mixture first forms a polyamic acid precursor. Upon heating at or above 300 C, the polyamic acids form polyimides, which are particularly suitable for use as a high temperature coating, adhesive, thin film, or composite matrix resin.

Ruth H Pater↗

Space Environmentally Durable Polyimides and Copolyimides

Polyimides displaying low color in thin films, atomic oxygen resistance, vacuum ultraviolet radiation resistance, solubility in organic solvents in the imide form, high glass transition (T(sub g)) temperatures, and high thermal stability are provided. The poly(amide acid)s, copoly(amide acid)s, polyimides and copolyimides are prepared by the reaction of stoichiometric ratios of an aromatic dianhydride with diamines which contain phenylphosphine oxide groups in polar aprotic solvents. Controlled molecular weight oligomeric (amide acid)s and imides can be prepared by offsetting the stoichiometry according to the Carothers equation using excess diamine and endcapping with aromatic anhydrides The polyimide materials can be processed into various material forms such as thin films, fibers, foams, threads, adhesive film, coatings, dry powders, and fiber coated prepreg, and uses include thin film membranes on antennas, second-surface mirrors, thermal optical coatings, and multilayer thermal insulation (MLI) blanket materials.

John W Connell↗

Low-Cost, High Glass-Transition Temperature, Thermosetting Polyimide Developed

PMR-15 polyimide, developed in the mid-1970's at the NASA Lewis Research Center, is recognized as a state-of-the-art high-temperature resin for composite applications in the temperature range of 500 to 550 F (260 to 288 C). PMR-15 offers easy processing and good property retention at a reasonable cost. For these reasons, it is widely used in both military and commercial aircraft engine components. Traditionally, polyimide composites have been designed for long-term use at 500 to 600 F over thousands of hours. However, new applications in reusable launch vehicles (RLV's) require lightweight materials that can perform for short times (tens of hours) at temperatures between 800 and 1000 F (425 and 538 C). Current efforts at Lewis are focused on raising the use temperature of polyimide composites by increasing the glass-transition temperature of the matrix resins. Achieving this dramatic increase in the upper use temperature without sacrificing polymer and composite processability is a major technical challenge.

Chuang, Kathy C.↗

Structural and Acoustic Damping Characteristics of Polyimide Microspheres

A broad range of tests have been performed to evaluate the capability of tiny lightweight polyimide spheres to reduce sound and vibration. The types of testing includes impedance tube measurement of propagation constant, sound power insertion loss for single and double wall systems, particle frame wave characterization and beam vibration reduction. The tests were performed using spheres made of two types of polyimide and with varying diameter. Baseline results were established using common noise reduction treatment materials such as fiberglass and foam. The spheres were difficult to test due to their inherent mobility. Most tests required some adaptation to contain the spheres. One test returned obvious non-linear behavior, a result which has come to be expected for treatments of this type. The polyimide spheres are found to be a competent treatment for both sound and vibration energy with the reservation that more work needs to be done to better characterize the non-linear behavior.

Palumbo, Daniel L.↗

Thermal Cycling of Thermal Control Paints on Carbon-Carbon and Carbon-Polyimide Composites

Carbon-carbon composites and carbon-polyimide composites are being considered for space radiator applications owing to their light weight and high thermal conductivity. For those radiator applications where sunlight will impinge on the surface, it will be necessary to apply a white thermal control paint to minimize solar absorptance and enhance infrared emittance. Several currently available white thermal control paints were applied to candidate carbon-carbon and carbon-polyimide composites and were subjected to vacuum thermal cycling in the range of -100 C to +277 C. The optical properties of solar absorptance and infrared emittance were evaluated before and after thermal cycling. In addition, adhesion of the paints was evaluated utilizing a tape test. The test matrix included three composites: resin-derived carbon-carbon and vapor infiltrated carbon-carbon, both reinforced with pitch-based P-120 graphite fibers, and a polyimide composite reinforced with T-650 carbon fibers, and three commercially available white thermal control paints: AZ-93, Z-93-C55, and YB-71P.

Jaworske, Donald A.↗

Polyimides from 2,3,3',4'-Biphenyltetracarboxylic Dianhydride and Aromatic Diamines

The present invention relates generally to polyimides. It relates particularly to novel polyimides prepared from 2,3, 3',4' -biphenyltetracarboxylic dianhydride and aromatic diamines. These novel polyimides have low color, good solubility, high thermal emissivity, low solar absorptivity and high tensile strength.

Hergenrother, Paul M.↗

Modified Single-Wall Carbon Nanotubes for Reinforce Thermoplastic Polyimide

A significant improvement in the mechanical properties of the thermoplastic polyimide film was obtained by the addition of noncovalently functionalized single-wall carbon nanotubes (SWNTs). Polyimide films were reinforced using pristine SWNTs and functionalized SWNTs (F-SWNTs). The tensile strengths of the polyimide films containing F-SWNTs were found to be approximately 1.4 times higher than those prepared from pristine SWNTs.

Lebron-COlon, Marisabel↗

Electron Beam Exposure of Thermal Control Paints on Carbon-Carbon and Carbon-Polyimide Composites

Carbon-carbon and carbon-polyimide composites are being considered for use as radiator face sheets or fins for space radiator applications. Several traditional white thermal control paints are being considered for the surface of the composite face sheets or fins. One threat to radiator performance is high energy electrons. The durability of the thermal control paints applied to the carbon-carbon and carbon-polyimide composites was evaluated after extended exposure to 4.5 MeV electrons. Electron exposure was conducted under argon utilizing a Mylar(TradeMark) bag enclosure. Solar absorptance and infrared emittance was evaluated before and after exposure to identify optical properties degradation. Adhesion of the paints to the carbon-carbon and carbon-polyimide composite substrates was also of interest. Adhesion was evaluated on pristine and electron beam exposed coupons using a variation of the ASTM D-3359 tape test. Results of the optical properties evaluation and the adhesion tape tests are summarized.

Jaworske, Donald A.↗

Space Environmentally Durable Polyimides and Copolyimides

Polyimides displaying low color in thin films, atomic oxygen resistance, vacuum ultraviolet radiation resistance, solubility in organic solvents in the imide form, high glass transition (T(sub g)) temperatures, and high thermal stability are provided. The poly(amide acid)s, copoly(amide acid)s, polyimides and copolyimides are prepared by the reaction of stoichiometric ratios of an aromatic &anhydride with diamines which contain phenylphosphine oxide groups in polar aprotic solvents. Controlled molecular weight oligomeric (amide acid)s and imides can be prepared by offsetting the stoichiometry according to the Carothers equation using excess diamine and endcapping with aromatic anhydrides. The polyimide materials can be processed into various material forms such as thin films, fibers, foams, threads, adhesive film, coatings, dry powders, and fiber coated prepreg, and uses include thin film membranes on antennas, second-surface mirrors, thermal optical coatings, and multilayer thermal insulation (MLI) blanket materials.

Connell, John W.↗

Fabrication of a Thermally Isolated and Pre-amplified Transistor Module with Polyimide Micro-wires for Cryogenic Detectors

For use in cryogenic applications such as bolometer and x-ray microcalorimeter arrays, pre-amplifying Junction Field Effect Transistors (JFETs) are often required for the readout electronics. The optimum operating temperature of the JFETs is 130 Kelvin while the cryogenic detectors operate in the milli-Kelvin range. Thus, the JFETs must be heated up but thermally isolated from the surrounding cryogenic instruments. In the past, the thermal isolation was accomplished by suspending the JFETs with low conductance wires such as manganium or stainless steel on a Kevlar support platform [I]. This also achieved electrical connections. However, this assembly required manual soldering work, which could raise a reliability issue for the cryogenic applications. In order to eliminate the manual work, polyimide micro-wires were developed [2]. The wires must be of sufficient length to decrease the heat load and in tension to prevent microphonic noise from vibration of the wires: the polyimide wires were patterned into llS"shaped curves over a thin metal wires such as aluminum, titanium, or niobium. The bilayer of the films were then suspended by etching silicon substrate thus to make freestanding air bridges (enough explanation?). In this paper, we present a method to fabricate micromachined JFET mechanical modules suspended by polyimide Pyraline micro-wires and heated up with built-in aluminum micro-heaters.

Oh, L. H.↗

Phenylated polyimides prepared from 3,6-diarylpyromellitic dianhydride and aromatic diamines

A new class of soluble phenylated polyimides made from 3,6-diarypyromellitic dianhydride and process for the manufacture of the 3,6-diarypyromellitic dianhydride starting material. The polyimides obtained with said dianhydride are readily soluble in appropriate organic solvents and are distinguished by excellent thermal, electrical and/or mechanical properties making the polyimides ideally suited as coating materials for microelectronic apparatii, as membranes for selective molecular separation or permeation or selective gas separation or permeation, or as reinforcing fibers in molecular composites, or as high modulus, high tensile strength fibers.

Harris, Frank W.↗

Electrically conductive polyimide film containing gold (III) ions, composition, and process of making

An electrically conductive, thermooxidatively stable poltimide, especially a film thereof, is prepared from an intimate admixture of a particular polyimide and gold (III) ions, in an amount sufficient to provide between 17 and 21 percent by weight of gold (III) ions, based on the weight of electrically conductive, thermooxidatively stable polyimide. The particular polyimide is prepared from a polyamic acid which has been synthesized from a dianhydride/diamine combination selected from the group consisting of 3,3',4,4'-benzophenonetetracarboxylic dianhydride and 2,2-bis[4-(4 -aminophenoxy)phenyl]hexafluoropropane; 3,3',4,4'-benzophenonetetracarboxylic dianhydride and 4,4'-oxydianiline; 2,2'-bis(3,4-dicarboxyphenyl)hexafluoropropane dianhydride and 4,4'-oxydianiline; and 3,3'4,4'-benzophenonetetracarboxylic dianhydride and 2,2-bis(3-aminophenyl)hexafluoropropane.

Caplan, Maggie L.↗

High-temperature polyimides prepared from 2,2-bis-[(2-halo-4-aminophenoxy)-phenyl]hexafluoropropane

There are provided the aromatic diamines 2,2-bis-[(2-halo-4-aminophenoxy)-phenyl]hexafluoropropane, where the attached ortho halogen is preferably chlorine, and 4,4'-bis(4-aminophenoxy)biphenyl, as novel monomers for polyimide polymerizations. The former, when reacted with 2,2-bis(3,4-dicarboxyphenyl)hexafluoropropane dianhydride, provides a polyimide having exceptional high-temperature performance. The latter diamine is a low-cost monomer for polyimide production.

Jones, Robert J.↗

Polyimides comprising substituted benzidines

A new class of polyimides and copolyimides made from substituted benzidines and aromatic dianhydrides and other aromatic diamines. The polyimides obtained with said diamines are distinguished by excellent thermal, excellent solubility, excellent electrical properties such as very low dielectric constants, excellent clarity and mechanical properties making the polyimides ideally suited as coating materials for microelectronic apparatii, as membranes for selective molecular or gas separation, as fibers in molecular composites, as high tensile strength, high compression strength fibers, as film castable coatings, or as fabric components.

Harris, Frank W.↗

Investigation of Aromatic/Aliphatic Polyimides as Dispersants for Single Wall Carbon Nanotubes

Novel aromatic/aliphatic polyimides were prepared from 2,7-diamino-9,9'- dioctylfluorene (AFDA) and aromatic dianhydrides. Upon investigating the effectiveness of these polyimides for dispersing single wall carbon nanotubes (SWNTs) in solution, three were discovered to disperse SWNTs in N,N-dimethylacetamide (DMAc). Two of these polyimides, one from 3,3',4,4'-oxydiphthalic anhydride (ODPA) and one from symmetric 3,3',4,4'-biphenyltetracarboxylic dianhydride (s-BPDA), were used to prepare nanocomposites. Homogeneous polyimide/SWNT suspensions from both polymers were used in the preparation of films and fibers containing up to 1 wt% SWNTs. The samples were thermally treated to remove residual solvent and the films were characterized for SWNT dispersion by optical and high resolution scanning electron microscopy (HRSEM). Electrical and mechanical properties of the films were also determined. Electrospun fibers were examined by HRSEM to characterize SWNT alignment and orientation.

Delozier, Donavon M.↗

Photochemically Synthesized Polyimides

An alternative to the conventional approach to synthesis of polyimides involves the use of single monomers that are amenable to photopolymerization. Heretofore, the synthesis of polyimides has involved multiple-monomer formulations and heating to temperatures that often exceed 250 C. The present alternative approach enables synthesis under relatively mild conditions that can include room temperature. The main disadvantages of the conventional approach are the following: Elevated production temperatures can lead to high production costs and can impart thermal stresses to the final products. If the proportions of the multiple monomeric ingredients in a given batch are not exactly correct, the molecular weight and other physical properties of the final material could be reduced from their optimum or desired values. To be useful in the alternative approach, a monomer must have a molecular structure tailored to exploit Diels-Alder trapping of a photochemically generated ortho-quinodimethane. (In a Diels-Alder reaction, a diene combines with a dienophile to form molecules that contain six-membered rings.) In particular, a suitable monomer (see figure) contains ortho-methylbenzophenone connected to a dienophile (in this case, a maleimide) through a generic spacer group. Irradiation with ultraviolet light gives rise to a photochemical intermediate the aforementioned ortho-quinodimethane from the ortho-methylbenzophenone. This group may react with the dienophile on another such monomer molecule to produce an oligomer that, in turn may react in a stepgrowth manner to produce a polyimide. This approach offers several advantages in addition to those mentioned above: The monomer can be stored for a long time because it remains unreactive until exposed to light. Because the monomer is the only active starting ingredient, there is no need for mixing, no concern for ensuring correct proportions of monomers, and the purity of the final product material is inherently high. The use of solvents is optional: The synthesis can be performed using the neat monomer or the monomer mixed with one or more solvent(s) in dilute or concentrated solution. The solubility of the monomer and the physical and chemical properties of the final polymer can be tailored through selection of the spacer group.

Meador, Michael A.↗

Improvements to the Synthesis of Polyimide Aerogels

Cross-linked polyimide aerogels are viable approach to higher temperature, flexible insulation for inflatable decelerators. Results indicate that the all-polyimide aerogels are as strong or stronger than polymer reinforced silica aerogels at the same density. Currently, examining use of carbon nanofiber and clay nanoparticles to improve performance. Flexible, polyimide aerogels have potential utility in other applications such as space suits, habitats, shelter applications, etc. where low dusting is desired

Meador, Mary Ann B.↗

Polyimide Foams Offer Superior Insulation

At Langley Research Center, Erik Weiser and his colleagues in the Advanced Materials and Processing Branch were working with a new substance for fabricating composites for use in supersonic aircraft. The team, however, was experiencing some frustration. Every time they tried to create a solid composite from the polyimide (an advanced polymer) material, it bubbled and foamed. It seemed like the team had reached a dead end in their research - until they had another idea. "We said, This isn t going to work for composites, but maybe we could make a foam out of it," Weiser says. "That was kind of our eureka moment, to see if we could go in a whole other direction. And it worked." Weiser and his colleagues invented a new kind of polyimide foam insulation they named TEEK. The innovation displayed a host of advantages over existing insulation options. Compared to other commercial foams, Weiser explains, polyimide foams perform well across a broad range of temperatures, noting that the NASA TEEK foams provide effective structural insulation up to 600 F and down to cryogenic temperatures. The foam does not burn or off-gas toxic fumes, and even at -423 F - the temperature of liquid hydrogen - the material stays flexible. The inventors could produce the TEEK foam at a range of densities, from 0.5 pounds per cubic foot up to 20 pounds per cubic foot, making the foam ideal for a range of applications, including as insulation for reusable launch vehicles and for cryogenic tanks and lines. They also developed a unique, friable balloon format for manufacturing the foam, producing it as hollow microspheres that allowed the foam to be molded and then cured into any desired shape - perfect for insulating pipes of different sizes and configurations. The team s originally unplanned invention won an "R&D 100" award, and a later form of the foam, called LaRC FPF-44 (Spinoff 2009), was named "NASA Invention of the Year" in 2007.

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