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At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
NASA NTRS1991

Polyimides containing pendent siloxane groups

The incorporation of siloxane units into the backbone of aromatic polyimides has been shown to impart certain advantages over the unmodified polyimides. These include enhanced solubility, lower moisture adsorption, lower dielectric constant, improved toughness and surface modification. Also, when exposed to an atomic oxygen environment these materials form an in-situ silicate (SiO2) surface coating which protects the underlying material from further erosion. These unique advantages make polyimide-siloxanes useful in a variety of electronic and aerospace applications. As part of an effort on high performance polymeric materials for potential aerospace applications, polyimides containing pendent siloxane groups are under study. These materials were prepared by reacting a functionalized siloxane compound with polyimides containing benzhydrol groups. Thin films of the polymers exhibited glass transition temperatures ranging from 167 to 235 C. Tensile strengths and moduli measured at 23 C ranged from 11 to 14 ksi and 250 to 450 ksi, respectively. The dielectric constant was lowered substantially from that of the unmodified polyimide.

Connell, John W.↗
NASA NTRS1995

Synthesis of low color, atomic oxygen resistant polyimides

The purpose of this project was to develop low color, atomic oxygen resistant polyimides for potential applications on spacecraft in low earth orbit. The material is needed in order to protect satellites and spacecraft from the gases and radiation found at those altitudes. Phosphorous containing polyimides have been shown to be especially resistant to corrosion and weight loss under oxygen plasma. Unfortunately the color of these phosphorous containing polyimides is still too high for them to be good heat insulators. While they are not as effective as teflon, the current material of choice. polyimides are much less dense than teflon and would be especially valuable if they could be made with low color. The approach taken was to synthesize a monomer which would contain the elements needed for giving the final polyimide its desired properties. In particular the monomer should incorporate phosphine or phosphine oxides and have bulky side groups to block any color forming charge transfer structures. The target molecule, 3,5-di-(trifluoromethylphenyl)-bis(3-aminophenyl) phosphine oxide, (containing both a phosphine oxide group and a bulky ditrifluoromethylphenyl group) was synthesized via three reactions in overall yield of 21 percent. In addition, a model compound, bis(3-phenylamine) phenyl phosphine oxide, was synthesized two different ways in order to establish the conditions for the nitration of phosphine oxides and their reduction to the amine. Finally, a trisubstituted phosphine oxide was synthesized. In all, seven phosphorus containing organic compounds were synthesized, purified and characterized. The model compound was reacted with oxydiphthalic anhydride to form a polyamic acid with inherent viscosity of 0.34. This material was cast into a film and heated, forming a normally colored fairly strong polyimide with a Tg of 240 C. The target compound was reacted with 6-fluorodiphthalic anhydride to give a polyamic acid with inherent viscosity of 0.19 and cast to give a heavily cracked colored film with a Tg of 230 C.

MacInnes, Dave↗
NASA NTRS1996

Effect of Temperature and Deformation Rate on the Tensile Mechanical Properties of Polyimide Films

In order to study the structure-property relationships of different processed oriented polyimide films, the mechanical properties will be identified by using tensile tester Instron 4505 and structural information such as the 3-dimensional birefringence molecular symmetry axis and 3-dimensional refractive indices will be determined by using wave guide coupling techniques. The monoaxial drawing techniques utilized in this research are very useful for improving the tensile mechanical properties of aromatic polyimide films. In order to obtain high modulus/high strength polyimide films the following two techniques have been employed, cold drawing in which polyimide films are drawn at room temperature at different cross head speeds and hot drawing in which polyimide films are drawn at different temperatures and cross head speeds. In the hot drawing process the polyimide films are drawn at different temperatures until the glass transition temperature (Tg) is reached by using the environmental chamber. All of the mechanical and optical property parameters will be identified for each sample processed by both cold and hot drawing techniques.

Moghazy, Samir F.↗
NASA NTRS2000

Aromatic Polyimide Foam

A mechanically undensified aromatic polyimide foam is made from an aromatic polyimide precursor solid residuum and has the following combination of properties: a density according to ASTM D-3574A of about 0.5 pounds/cu.ft to about 20 pounds/cu.ft; a compression strength according to ASTM D-3574C of about 1.5 psi to about 1500 psi; and a limiting oxygen index according to ASTM D-2863 of about 35% oxygen to about 75% oxygen at atmospheric pressure. The aromatic polyimide foam has no appreciable solid inorganic contaminants which are residues of inorganic blowing agents. The aromatic polyimide which constitutes the aromatic polyimide foam has a glass transition temperature (Tg) by differential scanning calorimetry of about 235 C to about 400 C; and a thermal stability of 0 to about 1% weight loss at 204 C as determined by thermogravinietric analysis (TGA). The aromatic polyimide foam has utility as foam insulation and as structural foam, for example, for aeronautical, aerospace and maritime applications.

Weiser, Erik S.↗
NASA NTRS1994

Negative birefringent polyimide films

A negative birefringent film, useful in liquid crystal displays, and a method for controlling the negative birefringence of a polyimide film is disclosed which allows the matching of an application to a targeted amount of birefringence by controlling the degree of in-plane orientation of the polyimide by the selection of functional groups within both the diamine and dianhydride segments of the polyimide which affect the polyimide backbone chain rigidity, linearity, and symmetry. The higher the rigidity, linearity and symmetry of the polyimide backbone, the larger the value of the negative birefringence of the polyimide film.

Harris, Frank W.↗
NASA NTRS2017

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. Furthermore, the new process allows us to tailor-make a high strength polymer that can be used to fabricate filament feedstock instead of pellets for 3D printing. The primary objective of this proposal is to determine the relationship between molecular structure, physical properties, and performance of ionic polyimides. Further, we seek to determine their utility as materials suitable for additive manufacturing of components used in aerospace vehicles, with an emphasis on characterizing and simulating their thermal behaviors and properties. This proposal addresses the need for fundamental research on a customizable polymer filament feedstock for 3-D printing with tailor-made properties potentially making it superior to the commercial blends offered in industry today. The deliverables for this project are the creation of a database that will detail the relationships between the molecular structure and physical properties for the ionic polyimide of interest (e.g. Tg/Tm (Glass Transition Temperature divided by Melting Point)) relative to different ionic polyimide structures). This new database will provide a “road map” to the development of the first generation of materials and ultimately proof-of-concept.

Jackson, Enrique↗
NASA NTRS1982

Tribological evaluation of composite materials made from a partially fluorinated polyimide

Preliminary tribological studies on a new polyimide formulated from the diamine 2,2-bis 4-(4-aminophenoxy) phenyl hexafluoropane (4-BDAF) indicates polyimides made from this diamine have excellent potential for high temperature applications. Two different polyimides were formulated from the diamine, and five different composites were formulated using one of the polyimides. Composites were made using 10 weight percent (w/o) graphite fluoride powder, 20 w/o PTFE powder, 30 w/o silver powder, or 50 w/o carbon fibers, both graphitic and nongraphitic types. The powder additions did not improve the tribological properties as much as the carbon fibers, and the graphitic fibers produced better results than did the nongraphitic fibers. Results also indicated that improved high temperature stability and tribological properties may be obtained with a polyimide made from the dianhydride pyromellitic acid (PMDA) rather than the dianhydride benzophenonetetracarboxylic acid (BTDA).

Fusaro, R. L.↗
NASA NTRS1982

Fundamental aspects of polyimide dry film and composite lubrication: A review

The tribological properties of polyimide dry films and composites are reviewed. Friction coefficients, wear rates, transfer film characteristics, wear surface morphology, and possible wear mechanisms of several different polyimide films, polyimide-bonded solid lubricants, polyimide solid bodies, and polyimide composites are discussed. Such parameters as temperature, type of atmosphere, load, contact stress, and specimen configuration are investigated. Data from an accelerated test device (Pin-on-Disk) are compared to similar data obtained from an end use application test device (plain spherical bearing).

Fusaro, R. L.↗
NASA NTRS1985

Optically transparent/colorless polyimides

Several series of linear aromatic polyimide films have been synthesized and characterized with the objective of obtaining maximum optical transparency. Two approaches have been used as part of this structure-property relationship study. The first approach is to vary the molecular structure so as to separate chromophoric centers and reduce electronic interactions between polymer chains to lower the intensity of color in the resulting polymer films. A second and concurrent approach is to perform polymerizations with highly purified monomers. Glass transition temperatures of thermally cured polyimide films are obtained by thermomechanical analysis and thermal decomposition temperatures are determined by thermogravimetric analysis. Transmittance UV-visible spectra of the polyimide films are compared to that of a commercial polyimide film. Fully imidized films are tested for solubility in common organic solvents. The more transparent films prepared in this study are evaluated for use on second-surface mirror thermal control coating systems. Lightly colored to colorless films are characterized by UV-visible spectroscopy before and after exposure to 300 equivalent solar hours UV irradiation and varying doses of 1 MeV electron irradiation. The effects of monomer purity, casting solvent and cure atmosphere on polyimide film transparency are also investigated.

Stclair, A. K.↗
NASA NTRS1986

Polyimides containing oxyethylene units. Part 4: Polymerization of dianhydrides containing ether linkages

The development of new composite resins for various aerospace applications is attempted. Although it is highly desirable that these polymers be soluble in order to facilitate processing, they must display considerable solvent-resistance in use. A recent approach has involved the synthesis of a new series of polyimides containing flexible linkages. The polymers were prepared by the polymerization of aromatic dianhydrides with diamines containing oxyethylene linkages. For example, the polymerization of 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) with 1,2-bis(4-aminophenoxy)ethane (1a) and bis2-(4-aminophenoxy)ethylether (lb), afforded highly crystalline polyimides that were completely insoluble. However, a polyimide that was amorphous and soluble was obtained from the polymerization of BTDA and an isomer of lb, i.e., bis2-(3-aminophenoxy)ethyl ether (4b). In an attempt to obtain a soluble, amorphous polyimide that could be annealed into a crysalline state, block copolymers of 1b and 4b and BTDA were prepared. Copolymers containing less than 20 weight % 1b were soluble in organic solvents. However, these polymers did not crystallize when heated above their Tg's. Copolymers containing higher levels of 1b were semicrystalline and insoluble. The polymerization of the diamines containing oxyethylene linkages with 4,4'-oxydiphthalic anhydride (ODPA) and a new dianhydride, i.e., 4,4'-oxyethyleneoxyethyleneoxydiphthalic anhydride (OEDA) was investigated. It was postulated that the use of these more flexible dianhydrides would result in more processable polyimides.

Harris, F. W.↗
NASA NTRS1987

Thermo-oxidatively stable condensation polyimides containing 1,1,1-triaryl-2,2,2-trifluoroethane dianhydride and diamine monomers

Nine new condensation polyimides containing the trifluorophenylethylidene linkage were synthesized by the amic-acid route. Several other polyimides, including some with the hexafluoroisopropylidene linkage, were also prepared as controls. Amic-acid solutions were characterized by determining their inherent viscosities prior to thermal conversion into polyimide films. Glass transition temperatures (T sug g), thermogravimetric analysis (TGA), and isothermal weight loss data were obtained for the films. The films were pulverized into molding powders which, in turn, were thermally processed under pressure into neat resin discs. The discs were also characterized by T sub gs and 316 C and 371 C isothermal weight losses. The film study identified two new polyimides with T sub gs greater that 371 C and two new polyimides with low rates of weight loss. The resin discs exhibited the same overall trends in T sub g and weight loss as the respective films, however the weight loss per unit surface area was always greater, presumably due to voids or to mechanical degradation induced during preparation of the molding powders.

Alston, William B.↗
NASA NTRS1988

Semi-interpenetrating polymer network's of polyimides: Fracture toughness

The objective was to improve the fracture toughness of the PMR-15 thermosetting polyimide by co-disolving LaRC-TPI, a thermoplastic polyimide. The co-solvation of a thermoplastic into a thermoset produces an interpenetration of the thermoplastic polymer into the thermoset polyimide network. A second research program was planned around the concept that to improve the fracture toughness of a thermoset polyimide polymer, the molecular weight between crosslink points would be an important macromolecular topological parameter in producing a fracture toughened semi-IPN polyimide.

Hansen, Marion Glenn↗
NASA NTRS1990

Autoclavable addition polyimides for 371 C composite applications

Studies were conducted to improve the thermo-oxidative stability (TOS) of PMR type polyimides by the substitution of para-aminostyrene (PAS) for the nadic ester endcap in second generation PMR polyimides (PMR-2). The nadic endcap which provides the PMR polyimides with their relative ease of fabrication, both by limiting the molecular weight of the prepolymer and by undergoing the final addition cure without volatiles, is also the weak link with regard to TOS. A polyimide formulated with PAS endcaps, called V-CAP, utilizes a two step reaction sequence similar to that of the PMR polyimides and can be easily autoclave molded into low void composite materials. Resin studies included two formulations of both PMR-2 and V-CAP, corresponding to n=9 and n=14 prepolymer stoichiometry. Unidirectional reinforced T40R graphite fiber laminates were fabricated from each of the resins was post-cured in either air at 385 C or nitrogen at 400 C. Composite specimens were aged in air at 371 C and mechanical properties were measured at 371 C before and after exposure.

Vannucci, R. D.↗
NASA NTRS1990

The mechanical stability of polyimide films at high pH

Polyimide insulated electrical wire has been widely used in the aerospace industry in commercial, military, and to a lesser degree, general aviation aircraft since the early 1970s. Wiring failures linked to insulation damage have drawn much attention in the media and concerns have developed regarding the long term stability and safety of polyimide insulated electrical wire. The mechanical durability and chemical stability of polyimide insulated wire are affected by hydrolysis, notch propagation, wet and dry arc tracking, topcoat flaking, and degradation due to high pH fluids. Several polyimides were selected for evaluation for resistance to degradation by various aqueous alkaline solutions. The polyimides under evaluation include commercially available films such as KAPTON (tradename), APICAL (tradename), LARC-TPI, and UPILEX (tradename) R and S, as well as a number of experimental films prepared at NASA-Langley. Material properties investigated include viscosity, solubility, moisture absorption, glass transition temperature, dielectric constant, and mechanical properties before and after exposure to various conditions.

Croall, Catharine I.↗
NASA NTRS1991

The effect of atomic oxygen on polysiloxane-polyimide for spacecraft applications in low Earth orbit

Polysiloxane-polyimide films are of interest as a replacement for polyimide Kapton in the Space Station Freedom solar array blanket. The blanket provides the structural support for the solar cells as well as providing transport of heat away from the back of the cells. Polyimide Kapton would be an ideal material to use; however, its high rate of degradation due to attack by atomic oxygen in low Earth orbit, at the altitudes Space Station Freedom will fly, is of such magnitude that if left unprotected, the blanket will undergo structural failure in much less than the desired 15 year operating life. Polysiloxane-polyimide is of interest as a replacement material because it should from its own protective silicon dioxide coating upon exposure to atomic oxygen. Mass, optical, and photomicrographic data obtained in the evaluation of the durability of polysiloxane-polyimide to an atomic oxygen environment are presented.

Rutledge, Sharon K.↗
NASA NTRS1990

Autoclavable addition polyimides for 371 C composite applications

Studies were conducted to improve the thermo-oxidative stability (TOS) of PMR type polyimides by the substitution of para-aminostyrene (PAS) for the nadic ester endcap in second generation PMR polyimides (PMR-2). The nadic endcap which provides the PMR polyimides with their relative ease of fabrication, both by limiting the molecular weight of the prepolymer and by undergoing the final addition cure without volatiles, is also the weak link with regard to TOS. A polyimide formulated with PAS endcaps, called V-CAP, utilizes a two step reaction sequence similar to that of the PMR polyimides and can be easily autoclave molded into low void composite materials. Resin studies included two formulations of both PMR-2 and V-CAP, corresponding to n = 9 and n = 14 prepolymer stoichiometry. Unidirectional reinforced T40R graphite fiber laminates were fabricated from each of the resins was post-cured in either air at 385 C or nitrogen at 400 C. Composite specimens were aged in air at 371 C and mechanical properties were measured at 371 C before and after exposure.

Vannucci, R. D.↗
NASA NTRS1993

High-Flow, High-Molecular-Weight, Addition-Curing Polyimides

In developed series of high-flow PMR-type polyimide resins, 2, 2'-bis(trifluoromethyl)-4, 4'-diaminobiphenyl (BTDB) substituted for 1, 4-pheylenediamine in PMR-II formulation. Polyimides designated either as PMR-12F when nadic ester (NE) end caps used, or as V-CAP-12F when p-aminostyrene end caps used. High-molecular-weight, addition-curing polyimides based on BTBD and HFDE highly processable high-temperature matrix resins used to make composite materials with excellent retention of properties during long-term exposure to air at 650 degrees F or higher temperature. Furthermore, 12F addition-curing polyimides useful for electronic applications; fluorinated rigid-rod polyimides known to exhibit low thermal expansion coefficients as well as low absorption of moisture.

Chuang, Kathy C.↗
NASA NTRS1995

The effect of simulated low earth orbit radiation on polyimides (UV degradation study)

UV degradation of polyimide films in air and vacuum were studied using UV-visible, ESR, FTIR, and XPS spectroscopies. The UV-visible spectra of polyimide films showed a blue shift in the absorption compared to Kapton. This behavior was attributed to the presence of bulky groups and kinks along the polymer chains which disrupt the formation of a charge transfer complex. The UV-visible spectra showed also that UV irradiation of polyimides result extensively in surface degradation, leaving the bulk of the polymer intact. ESR spectra of polyimides irradiated in vacuum revealed the formation of stable carbon-centered radicals which give a singlet ESR spectrum, while polyimides irradiated in air produced an asymmetric signal shifted to a lower magnetic field, with a higher g value and line width. This signal was attributed to oxygen-cenetered radicals of peroxy and/or alkoxy type. The rate of radical formation in air was two fold higher than for vacuum irradiation, and reached a plateau after a short time. This suggests a continuous depletion of radicals on the surface via an ablative degradation process. FTIR, XPS, and weight loss studies supported this postulate. An XPS study of the surface indicated a substantial increase in the surface oxidation after irradiation in air. The sharp increase in the C-O binding energy peak relative to the C-C peak was believed to be associated with an aromatic ring opening reaction.

Forsythe, John S.↗