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At least 847 records · Page 47

New High Temperature Cross Linking Monomers

This report describes the results of a one-year program designed to synthesize new, nonvolatile crosslinking monomers and to prove their feasibility in the development of lower temperature curing PMR-polyimide resins with high temperature capability. The objective of this program is to develop PMR-polyimide resins capable of being processed at a maximum temperature of 232C to 288C (450F to 500F) without sacrifice of the high temperature 316C (600F) capability of the state-of-the-art PMR-15 polyimide resin. Four monomethyl esters were synthesized and characterized for use in the crosslinking studies. It was found that all four crosslinkers were capable of entering into a crosslinking reaction to produce polymer specimens which were strong, dense and free of voids. The infrared and DSC studies of each crosslinker with monomers 4,4'-methylenedianiline (MDA) and the dimethyl ester of 3,3',4,4'-benzophenonetetracarboxylic acid (BTDE) comprising the resin systems, crosslinker/MDA/BTDE suggested that curing could be accomplished at 288C (550F). However, fabrication of dense, void free polymer specimens required a temperature of 316C (600F) and a pressure of 0.69 MPa (100 psi). The crosslinkers, monomethyl ester of 2,5-bicyclo[2.2.1]heptadiene-2,3-dicarboxylic acid (NDE) and monomethyl ester of maleic acid (MAE) were selected for evaluation in Celion 6000/PMR polyimide composites. These composites were characterized at RT, 288C (550F) and 316C (600F) initially and after isothermal aging at 288C (550F) and 316C (600F) for several hundred hours. The results of the isothermal aging studies suggested that both PMR systems NDE-MDA-BTDE and MAE-MDA-BTDE are promising candidates as matrices for addition type polyimide composites. These studies demonstrated that alternate crosslinkers to NE/MDA/BTDE are feasible, but mechanisms to lower the crosslinking temperature must be developed to provide lower temperature processing PMR-type polyimides.

Scola, Daniel A.↗

Flexible Microstrip Circuits for Superconducting Electronics

Flexible circuits with superconducting wiring atop polyimide thin films are being studied to connect large numbers of wires between stages in cryogenic apparatus with low heat load. The feasibility of a full microstrip process, consisting of two layers of superconducting material separated by a thin dielectric layer on 5 mil (approximately 0.13 mm) Kapton sheets, where manageable residual stress remains in the polyimide film after processing, has been demonstrated. The goal is a 2-mil (approximately 0.051-mm) process using spin-on polyimide to take advantage of the smoother polyimide surface for achieving highquality metal films. Integration of microstrip wiring with this polyimide film may require high-temperature bakes to relax the stress in the polyimide film between metallization steps.

Chervenak, James↗

High Temperature Resin Matrix Composites for Aerospace Structures

Accomplishments and the outlook for graphite-polyimide composite structures are briefly outlined. Laminates, skin-stiffened and honeycomb sandwich panels, chopped fiber moldings, and structural components were fabricated with Celion/LARC-160 and Celion/PMR-15 composite materials. Interlaminar shear and flexure strength data obtained on as-fabricated specimens and specimens that were exposed for 125 hours at 589 K indicate that epoxy sized and polyimide sized Celion graphite fibers exhibit essentially the same behavior in a PMR-15 matrix composite. Analyses and tests of graphite-polyimide compression and shear panels indicate that utilization in moderately loaded applications offers the potential for achieving a 30 to 50 percent reduction in structural mass compared to conventional aluminum panels. Data on effects of moisture, temperature, thermal cycling, and shuttle fluids on mechanical properties indicate that both LARC-160 and PMR-15 are suitable matrix materials for a graphite-polyimide aft body flap. No technical road blocks to building a graphite-polyimide composite aft body flap are identified.

Davis, J. G., Jr.↗

High-temperature resins

The basic chemistry, cure processes, properties, and applications of high temperature resins known as polyimides are surveyed. Condensation aromatic polymides are prepared by reacting aromatic diamines with aromatic dianhydrides, aromatic tetracarboxylic acids, or with dialkyl esters of aromatic tetracarboxylic acids, depending on the intended end use. The first is for coatings or films while the latter two are more suitable for polyimide matrix resins. Prepreg solutions are made by dissolving reactants in an aprotic solvent, and advances in the addition of a diamine on the double bond and radical polymerization of the double bond are noted to have yielded a final cure product with void-free characteristics. Attention is given to properties of the Skybond, Pyralin, and NR-150B polyimide prepreg materials and characteristics of aging in the NP-150 polyimides. Finally, features of the NASA-developed PMR polyimides are reviewed.

Serafini, T. T.↗

Development of an impact- and solvent-resistant thermoplastic composite matrix

Synthesis, moldability and chloroform, acetone and tricresyl phosphate resistance of 16 polymer compositions are described. These aliphatic heterocyclic polymers include polyimides, polybenzimidazoles, and N-arylenepolybenzimidazoles. A solution condensation (cresol) method to prepare imidized aliphaic polyimides is described. Two polyimides and one polybenzimidazole demonstrate no crazing or cracking during 500 hr exposure to the cited solvents under stress. Modification of one aliphatic polyimide with several aromatic amines suggests that m-phenylenediamine is singular in its behavior to improve the chloroform resistance of that class of polyimides.

Delano, C. B.↗

A tough performance simultaneous semi-interpenetrating polymer network

A semi-interpenetrating polyimide (semi-IPN) network and methods for making and using the same are disclosed. The semi-IPN system comprises a high performance thermosetting polyimide having an acetylene-terminated group acting as a crosslinking site and a high performance linear thermoplastic polyimide. The polymer is made by combining low viscosity precursors and low molecular weight polymers of the thermosetting and thermoplastic polyimides and allowing them to react in the immediate presence of each other to form a simultaneous semi-interpenetrating polyimide network. Provided is a high temperature system having significantly improved processability and damage tolerance while maintaining excellent thermo-oxidative stability, mechanical properties and resistance to humidity, when compared with the commercial high temperature resin, Thermid 600. This material is particularly adapted for use as a molding, adhesive and advanced composite matrix for aerospace structural and electronic applications.

Pater, Ruth H.↗

Microstructural Characterization of Semi-Interpenetrating Polymer Networks by Positron Lifetime Spectroscopy

Thermoset and thermoplastic polyimides have complementary physical and mechanical properties. Whereas thermoset polyimides are brittle and generally easier to process, thermoplastic polyimides are tough but harder to process. A combination of these two types of polyimides may help produce polymers more suitable for aerospace applications. Semi-Interpenetrating Polymer Networks (S-IPN) of thermoset LaRC(TM)-RP46 and thermoplastic LaRC(TM)-IA polyimides were prepared in weight percent ratios ranging from 100:0 to 0:100. Positron lifetime measurements were made in these samples to correlate their free volume features with physical and mechanical properties. As expected, positronium atoms are not formed in these samples. The second lifetime component has been used to infer the positron trap dimensions. The 'free volume' goes through a minimum at a ratio of about 50:50, and this suggests that S-IPN samples are not merely solid solutions of the two polymers. These data and related structural properties of the S-IPN samples are discussed.

Singh, Jag J.↗

Nuclear Instruments and Methods in Physics Research: Microstructural Characterization of Semi-Interpenetrating Polymer Networks by Positron Lifetime Spectroscopy - Section B

Thermoset and thermoplastic polyimides have complementary physical/mechanical properties. Whereas thermoset polyimides are brittle and generally easier to process, thermoplastic polyimides are tough but harder to process. It is expected that a combination of these two types of polyimides may help produce polymers more suitable for aerospace applications. Semi-Interpenetrating Polymer Networks (S-IPNs) of thermoset LaRC(Trademark)-RP46 and thermoplastic LARC(Trademark)-IA polyimides were prepared in weight percent ratios ranging from 100:0 to 0: 100. Positron lifetime measurements were made in these samples to correlate their free volume features with physical/mechanical properties. As expected, positronium atoms are not formed in these samples. The second life time component has been used to infer the positron trap dimensions. The "free volume" goes through a minimum at about 50:50 ratio, suggesting that S-IPN samples are not merely solid solutions of the two polymers. These data and related structural properties of the S-IPN samples have been discussed in this paper.

Singh, Jag J.↗

Composition and Process for Retarding the Premature Aging of PMR Monomer Solutions and PMR Prepegs

Polyimides are derived from solutions of at least one low-boiling organic solvent, e.g. isopropanol containing a mixture of polyimide-forming monomers. The monomeric solutions have an extended shelf life at ambient (room) temperatures as high as 80 C, and consist essentially of a mixture of monoalkyl ester-acids, alkyl diester-diacids and aromatic polyamines wherein the alkyl radicals of the esteracids are derived from lower molecular weight aliphatic secondary alcohols having 3 to 5 carbon atoms per molecule such as isopropanol, secondary butanol, 2-methyl-3-butanol, 2 pentanol or 3-pentanol. The solutions of the polyimide-forming monomers have a substantially improved shelf-life and are particularly useful in the aerospace and aeronautical industry for the preparation of polyimide reinforced fiber composites such as the polyimide cured carbon composites used in jet engines, missiles, and for other high temperature applications.

Alston, William B.↗

Surface Evaluation by XPS of High Performance Foams After Exposure to Oxygen Plasma

This report will present the results of a study done during a 10-week summer faculty fellowship during the summer of 2001 working with Ms. Martha Williams of the Testbeds Group at Kennedy Space Center. The work was in a new area for this faculty and was both interesting and enjoyable. An imide is a compound in which nitrogen is bonded directly to an R group and to two other R groups through carbonyls. Polyimides have a number of properties that make them highly desirable materials for use on structures that are exposed to extreme conditions. They are strong, fire resistant, minimally outgasing, stable over a large temperature range, resistant to chemical attack, transparent to infrared and microwaves, and have a low density. One polyimide, solimide, commercially available as a foam, retains resiliency from -300 F to +500 F, is highly flame retardant, and decomposes with virtually no smoke or toxic byproduct formation. The density of this product is such that its use in place of fiberglass in the lower lobe of a 747 saves 400 lb. Shipboard applications have resulted in literally tons of weight reduction. While polyimide films have been used in structures to be placed in low earth orbit (LEO) for many years, polyimide foams have found only minimal application in this realm. NASA Langley Research Center has developed new technology that allows for the processing of new polyimide foams. The resulting increased availability of these materials, along with their highly desirable properties, has prompted a study to determine the suitability of these materials for use in structures to be placed in LEO.

Hampton, Michael D.↗

Thin Film...Large Payoff

SRS Technologies is currently the only company licensed by Langley Research Center to produce colorless polyimides. They currently produce two polyimides, the LaRC-CP1 and LaRC-CP2 developed by Langley Research Center. These polyimides offer many advantages over other commercially available materials including excellent thermal stability, radiation resistance, solubility, and transparency. The SRS polyimides can be used in laminates, films, molded parts, and stock shapes. The polyimide technology has also helped the company further their development of solar arrays.

Source record↗

Research to Significantly Enhance Composites Survivability at 550 F in Oxidative Environments

Methylene dianiline (MDA) and its derivatives have been used in the synthesis of polyimides to yield polymers with characteristic low-density, high tensile strength, improved solubility in organic solvents, low-melt viscosities and high thermal stability (greater than 550 F) in air. Polyimides with such properties are desirable for use in aerospace systems, e.g., jet engines, airframe, missiles, and rockets where weight is critical. Recent research at Prairie View A&M University is focused on developing monomers to generate polyimides with enhanced performance over that of NASA s PMR-15. The objective of this work is to synthesize three ring aromatic diamines which are non-toxic and when reacted with the appropriate dianhydrides will yield polyimides with lower viscosity, improve processability, good retention of mechanical properties, and oxidative stability at high environmental temperatures. Modifications of the three ring aromatic diamines include replacing the methylene linkages with aromatic ethers by nucleophilic aromatic substitution reactions and incorporating mono- and di-substituents to the center aromatic ring. An update of current reactions involved in synthesis efforts to generate three ring aromatic monomers for polyimides with methylene, carbonyl, and ether linkages separating the aromatic moieties will be displayed.

Meador, Michael A.↗

Environmental Influence of Gravity and Pressure on Arc Tracking of Insulated Wires Investigated

Momentary short-circuit arcs between a defective polyimide-insulated wire and another conductor may thermally char (pyrolize) the insulating material. The charred polyimide, being conductive, can sustain the short-circuit arc, which may propagate along the wire through continuous pyrolization of the polyimide insulation (arc tracking). If the arcing wire is part of a multiple-wire bundle, the polyimide insulation of other wires within the bundle may become thermally charred and start arc tracking also (flash over). Such arc tracking can lead to complete failure of an entire wire bundle, causing other critical spacecraft or aircraft failures. Unfortunately, all tested candidate wire insulations for aerospace vehicles were susceptible to arc tracking. Therefore, a test procedure was designed at the NASA Lewis Research Center to select the insulation type least susceptible to arc tracking. This test procedure addresses the following three areas of concern: (1) probability of initiation, (2) probability of reinitiation (restrike), and (3) extent of arc tracking damage (propagation rate). Item 2 (restrike probability) is an issue if power can be terminated from and reapplied to the arcing wire (by a switch, fuse, or resettable circuit breaker). The degree of damage from an arcing event (item 3) refers to how easily the arc chars nearby insulation and propagates along the wire pair. Ease of nearby insulation charring can be determined by measuring the rate of arc propagation. Insulation that chars easily will propagate the arc faster than insulation that does not char very easily. A popular polyimide insulated wire for aerospace vehicles, MIL-W-81381, was tested to determine a degree of damage from an arcing event (item 3) in the following three environments: (1) microgravity with air at 1-atm pressure, (2) 1g with air at 1 atm, and (3) 1g within a 10^-6 Torr vacuum. The microgravity 1-atm air was the harshest environment, with respect to the rate of damage of arc tracking, for the 20 AWG (American Wiring Gauge) MIL-W-81381 wire insulation type . The vacuum environment resulted in the least damage. Further testing is planned to determine if the environmental results are consistent between insulation types and to evaluate the other two parameters associated with arc tracking susceptibility.

Source record↗

Prediction of Mechanical Properties of Polymers With Various Force Fields

The effect of force field type on the predicted elastic properties of a polyimide is examined using a multiscale modeling technique. Molecular Dynamics simulations are used to predict the atomic structure and elastic properties of the polymer by subjecting a representative volume element of the material to bulk and shear finite deformations. The elastic properties of the polyimide are determined using three force fields: AMBER, OPLS-AA, and MM3. The predicted values of Young s modulus and shear modulus of the polyimide are compared with experimental values. The results indicate that the mechanical properties of the polyimide predicted with the OPLS-AA force field most closely matched those from experiment. The results also indicate that while the complexity of the force field does not have a significant effect on the accuracy of predicted properties, small differences in the force constants and the functional form of individual terms in the force fields determine the accuracy of the force field in predicting the elastic properties of the polyimide.

Odegard, Gregory M.↗

Substituted Cyclohexene Endcaps for Polymers with Thermal-Oxidative Stability

This invention relates to polyimides having improved thermal-oxidative stability, to the process of preparing said polyimides, and the use of polyimide prepolymers in the preparation of prepregs and composites. The polyimides are particularly usefull in the preparation of fiber-reinforced, high-temperature composites for use in various engine parts including inlets, fan ducts, exit flaps and other parts of high speed aircraft. The polyimides are derived from the polymerization of effective amounts of at least one tetracarboxylic dianhydride, at least one polyamine and a novel dicarboxylic endcap having the formula presented.

Source record↗

Fiber reinforced thermoplastic resin matrix composites

Polyimide polymer composites having a combination of enhanced thermal and mechanical properties even when subjected to service temperatures as high as 700.degree. F. are described. They comprise (a) from 10 to 50 parts by weight of a thermoplastic polyimide resin prepared from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane and (b) from 90 to 50 parts by weight of continuous reinforcing fibers, the total of (a) and (b) being 100 parts by weight. Composites based on polyimide resin formed from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane and pyromellitic dianhydride and continuous carbon fibers retained at least about 50% of their room temperature shear strength after exposure to 700.degree. F. for a period of 16 hours in flowing air. Preferably, the thermoplastic polyimide resin is formed in situ in the composite material by thermal imidization of a corresponding amide-acid polymer prepared from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane. It is also preferred to initially size the continuous reinforcing fibers with up to about one percent by weight of an amide-acid polymer prepared from 2,2-bis[4-(4-aminophenoxy)phenyl]hexafluoropropane. In this way imidization at a suitable elevated temperature results in the in-situ formation of a substantially homogeneous thermoplastic matrix of the polyimide resin tightly and intimately bonded to the continuous fibers. The resultant composites tend to have optimum thermo-mechanical properties.

Jones, Robert J.↗

Tribological Evaluation of Candidate Gear Materials Operating Under Light Loads in Highly Humid Conditions

A series of pin-on-disk sliding wear tests were undertaken to identify candidate materials for a pair of lightly loaded timing gears operating under highly humid conditions. The target application involves water purification and thus precludes the use of oil, grease and potentially toxic solid lubricants. The baseline sliding pair is austenitic stainless steel operating against a carbon filled polyimide. The test load and sliding speed (4.9N, 2.7ms) were chosen to represent average contact conditions of the meshing gear teeth. In addition to the baseline materials, the hard superelastic NiTiNOL 60 (60NiTi) was slid against itself, against the baseline polyimide, and against 60NiTi onto which a commercially deposited dry film lubricant (DFL) was applied. The alternate materials were evaluated as potential replacements to achieve a longer wear life and improved dimensional stability for the timing gear application. An attempt was also made to provide solid lubrication to self-mated 60NiTi by rubbing the polyimide against the disk wear track outside the primary 60NiTi-60NiTi contact, a method named stick or transfer-film lubrication. The selected test conditions gave repeatable friction and wear data and smooth sliding surfaces for the baseline materials similar to those in the target application. Friction and wear for self-mated stainless steel were high and erratic. Self-mated 60NiTi gave acceptably low friction (0.2) and modest wear but the sliding surfaces were rough and potentially unsuitable for the gear application. Tests in which 60NiTi pins were slid against DFL coated 60NiTi and DFL coated stainless steel gave low friction and long wear life. The use of stick lubrication via a secondary polyimide pin provided effective transfer film lubrication to self-mated 60NiTi tribological specimens. Using this approach, friction levels were equal or lower than the baseline polyimide-stainless combination and wear was higher but within data scatter observed in these preliminary tests. Based upon these results, self-mated 60NiTi gear teeth utilizing solid lubrication, is a reasonable approach for the target application.

tribology↗

Tribological Evaluation of Candidate Gear Materials Operating Under Light Loads in Highly Humid Conditions

A series of pin-on-disk sliding wear tests were undertaken to identify candidate materials for a pair of lightly loaded timing gears operating under highly humid conditions. The target application involves water purification and thus precludes the use of oil, grease and potentially toxic solid lubricants. The baseline sliding pair is austenitic stainless steel operating against a carbon filled polyimide. The test load and sliding speed (4.9 N, 2.7 m/s) were chosen to represent average contact conditions of the meshing gear teeth. In addition to the baseline materials, the hard superelastic NiTiNOL 60 (60NiTi) was slid against itself, against the baseline polyimide, and against 60NiTi onto which a commercially deposited dry film lubricant (DFL) was applied. The alternate materials were evaluated as potential replacements to achieve a longer wear life and improved dimensional stability for the timing gear application. An attempt was also made to provide solid lubrication to self-mated 60NiTi by rubbing the polyimide against the disk wear track outside the primary 60NiTi-60NiTi contact, a method named stick or transfer-film lubrication. The selected test conditions gave repeatable friction and wear data and smooth sliding surfaces for the baseline materials similar to those in the target application. Friction and wear for self-mated stainless steel were high and erratic. Self-mated 60NiTi gave acceptably low friction (approx. 0.2) and modest wear but the sliding surfaces were rough and potentially unsuitable for the gear application. Tests in which 60NiTi pins were slid against DFL coated 60NiTi and DFL coated stainless steel gave low friction and long wear life. The use of stick lubrication via the secondary polyimide pin provided effective transfer film lubrication to self-mated 60NiTi tribological specimens. Using this approach, friction levels were equal or lower than the baseline polyimide-stainless combination and wear was higher but within data scatter observed in these preliminary tests. Based upon these results, self-mated 60NiTi gear teeth utilizing solid lubrication, is a reasonable approach for the target application.

tribology↗