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At least 253 records · Page 14

Process for preparing an assembly of an article and a polyimide which resists dimensional change, delamination and debonding when exposed to changes in temperature

An assembly of an article and a polyimide composition is prepared. The assembly resists dimensional change, delamination, or debonding when exposed to changes in temperature. An article is provided. A polyamic acid solution which yields a polyimide having a low coefficient of thermal expansion (CTE) was prepared. Equimolar quantities of an aromatic diamine and an aromatic dianhydride were reacted in a solvent medium to form a polyamic acid solution. A metal ion-containing additive was added to the solution. Examples of this additive are: TbCl3, DyCl3, ErCl3, TmCl3, Al(C5H7O2)3, and Er2S3. The polyamic acid solution was imidized and is combined with the article to form the assembly.

Stoakley, Diane M.↗

Molecular beam scattering from C-13 enriched Kapton and correlation with the EOIM-3 carousel experiment

Mass spectra of products emerging from identical samples of a C-13-enriched polyimide polymer (chemically equivalent to Kapton) under atomic oxygen bombardment in space and in the laboratory were collected. Reaction products unambiguously detected in space were CO-13, NO, (12)CO2, and (13)CO2. These reaction products and two others, H2O and CO-12, were detected in the laboratory, along with inelastically scattered atomic and molecular oxygen. Qualitative agreement was seen in the mass spectra taken in space and in the laboratory; the agreement may be improved by reducing the fraction of O2 in the laboratory molecular beam. Both laboratory and space data indicated that CO and CO2 products come preferentially from reaction with the imide component of the polymer chain, raising the possibility that the either component may degrade in part by the 'evaporation' of higher molecular weight fragments. Laboratory time-of-flight distributions showed: (1) incomplete energy accommodation of impinging O and O2 species that do not react with the surface; and (2) both hyperthermal and thermal CO and CO2 products, suggesting two distinct reaction mechanisms with the surface.

Minton, Timothy K.↗

Processing and properties of fiber reinforced polymeric matrix composites: I. IM7/LARC(TM)-PETI-7 polyimide composites

A phenylethynyl terminated imide oligomer formed from the reaction of benzophenone tetracarboxylic acid dianhydride, an 75:25 molar ratio of 4,4'-oxydianiline and meta-phenylenediamine and 4-phenylethynylphthalic anhydride as the endcapper at a theoretical number average molecular weight (Mn) of approximately 3,700 g/mol was evaluated as a composite resin matrix. A glass transition temperature (Tg) of 315 deg C was reached after 250 deg C/1 hr annealing of the matrix resin. Unidirectional prepreg was made by coating an N-methylpyrrolidinone solution of the amide acid oligomer onto unsized IM7 graphite fibers. The thermal and rheological properties and the solvent/volatile depletion rates of the amide acid/NMP system were determined. This information was used to successfully design a molding cycle for composite fabrication. Composites molded under 800 Psi at 371 C consistently yielded good consolidation as measured by C-scan and optical photomicrography. The composite's short beam shear strength (SBS), longitudinal and transverse flexural strengths and moduli were measured at various temperatures. These composites exhibited excellent room temperature (RT) longitudinal flexural strength and modulus and RT SBS strength retention at 177 C.

Hou, Tan-Hung↗

Processing and Properties of Fiber Reinforced Polymeric Matrix Composites: Processing Robustness of IM7/PETI Polyimide Composites - Part 2

The processability of a phenylethynyl terminated imide (PETI) resin matrix composite was investigated. Unidirectional prepregs were made by coating an N-methylpyrrolidone solution of the amide acid oligomer onto unsized IM7. Two batches of prepregs were used: one was made by NASA in-house, and the other was from an industrial source. The composite processing robustness was investigated with respect to the effect of B-staging conditions, the prepreg shelf life, and the optimal processing window. Rheological measurements indicated that PETI's processability was only slightly affected over a wide range of B-staging temperatures (from 250 C to 300 C). The open hole compression (OHC) strength values were statistically indistinguishable among specimens consolidated using various B-staging conditions. Prepreg rheology and OHC strengths were also found not to be affected by prolonged (i.e., up to 60 days) ambient storage. An optimal processing window was established using response surface methodology. It was found that IM7/PETI composite is more sensitive to the consolidation temperature than to the consolidation pressure. A good consolidation was achievable at 371 C/100 Psi, which yielded an OHC strength of 62 Ksi at room temperature. However, processability declined dramatically at temperatures below 350 C.

Hou, Tan-Hung↗

Experiments Related to the Fabrication of Carbon Fiber/AMB-21 Polyimide Composite Tubes Using the RTM Process

AMB-21 is a new polymer developed by Mr. Ray Vannucci, NASA, LeRC as a noncarcinogenic polyimide matrix which may be suitable for fabricating composite parts by the Resin Transfer Modeling (RTM) process. The polyimide for this project was prepared at the Center of Composite Materials Research at N.C. A&T State University because it is not currently an item of commerce. The RTM process is especially suitable for producing geometrically complex composite parts at a low cost. Because of the high melting point and very high viscosity at the time of processing, polyimides have not been extensively used in the RTM process. The process for preparing AMB-21 as well as the process for fabricating composite plates will be described. The basic fabrication process consists of injecting a solvent solution of AMP-21 into a carbon fiber preform, evaporating the solvent, imidizing the polyimide, and vacuum/compression modeling the impregnated preform. All the above molding steps are preformed in a specially designed RTM mold which will be described. The results of this process have been inconsistent. Where as some experiments have resulted in a reasonably sound panels, others have not. Further refinements of the process are required to establish a reliable process.

Exum, Daniel↗

Tough, Soluble, Aromatic, Thermoplastic Copolyimides

Tough, soluble, aromatic, thermoplastic copolyimides were prepared by reacting 4,4'-oxydiphthalic anhydride, 3,4,3',4'-biphenyltetracarboxylic dianhydride and 3,4'-oxydianiline. These copolyimides were found to be soluble in common amide solvents such as N,N'-dimethyl acetamide, N-methylpyrrolidinone, and dimethylformamide allowing them to be applied as the fully imidized copolymer and to be used to prepare a wide range of articles.

Bryant, Robert G.↗

Effects of Heat Treatment on the Magnetic Properties of Polymer-Bound Iron Particle Cores

Spherical iron particles of three different size distributions, 6-10 micrometers in diameter, 100 mesh and 30-80 mesh, were mixed with 2.0 wt % of soluble imide and compression molded at 300 C under 131 MPa. Post-fabrication heat treatments were performed at 960 C for 6 h resulting in a significant enhancement of the permeability in low field region for all the specimens except for the one made of 30-80 mesh particles. The rate of core loss of these specimens at a magnetic induction of 5 kG measured up to 1 kHz shows a noticeable. increase after heat treatment which, along with the permeability enhancement, can be explained by the coalescence of particles forming a network of conductivity paths in the specimens. ne scanning electron micrographs taken for the 6-10 micrometer particle specimens show no evidence of heat treatment-induced grain growth. The untreated specimens show a very weak f(sup 2) -dependence of the core loss which clearly indicates a negligible contribution from the eddy current loss. In particular, an almost perfect linearity was found in the frequency dependence of the core loss of the untreated specimen made of 100 mesh iron particles.

Namkung, M.↗

Studies of Matrix/Fiber Reinforced Composite Materials for the High Speed Research (HSR) Program

The research on the curing mechanism of the phenylethynyl terminated imide matrix resins was the primary focus of this research. The ability to process high performance polymers into useful adhesives and high quality composites has been significantly advanced by synthetic techniques in which oligomers terminated with reactive groups cure or crosslink at elevated temperature after the article has been fabricated. The research used a variety of analytical techniques. Many stable products were isolated, and attempts at identification were made. This research was intended to provide fundamental insight into the molecular structure of these new engineering materials.

Orwoll, Robert A.↗

Synthesis and Characterization of Processable Polyimides with Enhanced Thermal Stability

The following is a summary report of the research carried out under NASA Grant NAG-1-448. The work was divided into four major areas: 1) Enhanced polyimide processing through the use of reactive plasticizers 2) Development of processable polyhenylquinoxalines 3) Synthesis and characterization of perfluorovinylether-terminated imide oligomers and 4) Fluorosilicones containing perfuorocyclobutane rings.

Harris, Frank W.↗

High Temperature Transfer Molding Resins

High temperature resins containing phenylethynyl groups that are processable by transfer molding have been prepared. These phenylethynyl containing oligomers were prepared from aromatic diamines containing phenylethynyl groups and various ratios of phthalic anhydride and 4-phenylethynlphthalic anhydride in glacial acetic acid to form a mixture of imide compounds in one step. This synthetic approach is advantageous since the products are a mixture of compounds and consequently exhibit a relatively low melting temperature. In addition, these materials exhibit low melt viscosities which are stable for several hours at 210-275 C, and since the thermal reaction of the phenylethynyl group does not occur to any appreciable extent at temperatures below 300 C, these materials have a broad processing window. Upon thermal cure at approximately 300-350 C, the phenylethynyl groups react to provide a crosslinked resin system. These new materials exhibit excellent properties and are potentially useful as adhesives, coatings, films, moldings and composite matrices.

Connell, John W.↗

Molecular Level Coating for Metal Oxide Particles

Polymer encapsulated metal oxide particles are prepared by combining a polyamide acid in a polar aprotic solvent with a metal alkoxide solution. The polymer was imidized and the metal oxide formed simultaneously in a refluxing organic solvent. The resulting polymer-metal oxide is an intimately mixed commingled blend, possessing synergistic properties of both the polymer and preceramic metal oxide. The encapsulated metal oxide particles have multiple uses including, being useful in the production of skin lubricating creams, weather resistant paints, as a filler for paper, making ultraviolet light stable filled printing ink, being extruded into fibers or ribbons, and coatings for fibers used in the production of composite structural panels.

McDaniel, Patricia R.↗

Films, Preimpregnated Tapes and Composites Made from Polyimide "Salt-Like" Solutions

High quality films, preimpregnated tape (prepegs), and composites have been fabricated from polyimide precursor 'saltlike' solutions. These salt-like solutions have a low viscosity (5,000 to 10,000 cp) and a high solids content (50-65% by weight) and can be coated onto reinforcing fiber to produce prepegs with excellent tack and drape at 12-15% residual solvent (approximately 4-6% water from thermal imidization reaction). The processing of these types of prepegs significantly overcomes solvent removal problems and allows excellent fiber wet out. In addition, the physical characteristics of the polyimide precursor salt-like solutions permits processing into high-performance materials through the use of standard prepregging and composite fabrication equipment. The resultant composites are of high quality.

Cano, Roberto J.↗

Zr-Containing 4,4'-ODA/PMDA Polyimide Composites

The objective of this research is to improve the atomic oxygen resistance of Kapton(TM), a polyimide (PI) made from pyromellitic acid dianhydride (PMDA) and 4,4'-oxydianiline (ODA), while retaining or enhancing the desirable properties of the pure polymer. Toward this end, zirconium-containing complexes and polymers were used to make composites and blends. Tetra(acetylacetonato)zirconium(IV), Zr(acac)4, which is commercially available, was identified as the best zirconium-containing complex for enhancing the atomic oxygen resistance of polyimide composites of the 10 complexes screened. Films prepared from the commercially available polyamic acid (PAA) of PMDA-ODA (DuPont) have good uniformity, flexibility, and tensile strength. A 24-layer 10% (mol) Zr(acac)4/PI composite film showed significant improvement (ca. 20 fold) of atomic oxygen resistance over the pure polyimide. However, 10% (mol) Zr(acac)4 represents an upper concentration limit, above which films undergo cracking upon thermal imidization. In order to increase the Zr complex concentration in PMDA-ODA PI films, while retaining good film properties, [Zr(adsp)2-PMDA]n coordination polymer [bis(4-amino-N,N'-disalicylidene- 1,2-phenylenediamino)zirconium(IV)-pyromellitic dianhydride] and [Zr(adsp)2-PMDA-ODA-PMDA]n terpolymer were synthesized and blended with commercial PAA, respectively. Several techniques were used to characterize the films made from the polymer containing Zr(acac)4. Plasma studies of films having 2% (mol) incremental concentrations of Zr in the Kapton up to 10% (mol) show that the overall rate of erosion is reduced about 75 percent.

Illingsworth, M. L.↗

Polyimide Based Nanocomposites for Affordable Space Transport

In setting forth its strategic plan, NASA has indicated that low-cost access to space is the key to unleashing the commercial potential of space and greatly expanding space research and exploration. The development of advanced materials will be an enabling technology for this quest for low-cost space access. In this research program, we are attempting to address the need for new advanced materials by developing high-performance nanodispersed inorganic/organic and organic/organic polyimide composites utilizing specific interactions. Our goal is to systematically manipulate these interactions and investigate the resulting processing morphology-property relationships. Specifically, we will investigate three main parameters on these relationships. These include (1) the type of polyimide; (2) the structure of the inorganic nanoparticle being used; and (3) manipulation of the interfacial energy. During the first year of this effort, we have demonstrated the successful synthesis of PMR-15/layered silicate nanocomposites. Morphological studies indicate that exfoliated structures were obtained in most instances, with a mixture of exfoliated and intercalated structures being observed also. Significant enhancements of the onset of decomposition were obtained by varying the strength of the interaction between the nanoparticle and the polymer. Varying the amount of a specific nanoparticle also affected the decomposition temperatures. A slight catalytic effect of the nanoparticles on both the imidization and crosslinking reaction has been observed and will be presented. In addition, incorporation of the nanoparticles was found to increase the glass transition temperature and slightly broaden the breadth of this relaxation.

Dean, Derrick↗

Phenylethynyl Containing Reactive Additives

Phenylethynyl containing reactive additives were prepared from aromatic diamines containing phenylethynyl groups and various ratios of phthalic anhydride and 4-phenylethynylphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pyrrolidinone to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.

John W Connell↗

Automated Tow Placed LaRC(TM)-PETI-5 Composites

LaRC(TM)-PETI-5 is a PhenylEthynyl-Terminated Imide resin developed at NASA Langley Research Center (LaRC) during the 1990s. It offers a combination of attractive composite and adhesive properties. IM7/LaRC(TM)-PETI-5 composites exhibit thermal and thermo-oxidative stability typical of polyimides, superior chemical resistance and processability, excellent mechanical properties, toughness and damage tolerance. It was selected for study in the High Speed Research program aimed at developing technologies for a future supersonic aircraft, the High Speed Civil Transport, with a projected life span of 60 000 h at a cruise speed up to Mach 2.4. Robust autoclave processing cycles for LaRC(TM)-PETI-5 composites have been thoroughly designed and demonstrated, which involved hand lay-up of solvent-ladened 'wet' prepregs. However, this type of processing is not only costly but also environmentally unfriendly. Volatile management and shrinkage could become serious problems in the fabrication of large complex airframe structural subcomponents. Robotic tow placement technology utilizing 'dry' material forms represents a new fabrication process which overcomes these deficiencies. This work evaluates and compares mechanical properties of composites fabricated by heated head automated tow placement (dry process) with those obtained by hand lay-up/autoclave fabrication (wet process). Thermal and rheological properties of the robotically as-placed uncured composites were measured. A post-cure cycle was designed due to the requirement of the PETI-5 resin for a 370 C/1 h hold to reach full cure, conditions which cannot be duplicated during heated head robotic placement. Mechanical properties such as 0 degree flexural strength and modulus, open hole tensile and compressive strength and moduli, reduced section compression dogbone compressive strength, and modified zippora-medium small (MZ-MS) tensile and compressive properties were obtained on the post-cured panels. These properties compared favourably with those obtained from the wet process.

Hou, T. H.↗

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.↗

Molecular Level Coating of Metal Oxide Particles

Polymer encapsulated metal oxide particles are prepared by combining a polyamide acid in a polar osmotic solvent with a metal alkoxide solution. The polymer was imidized and the metal oxide formed simultaneously in a refluxing organic solvent. The resulting polymer-metal oxide is an intimately mixed commingled blend, possessing, synergistic properties of both the polymer and preceramic metal oxide. The encapsulated metal oxide particles have multiple uses including, being useful in the production of skin lubricating creams, weather resistant paints, as a filler for paper. making ultraviolet light stable filled printing ink, being extruded into fibers or ribbons, and coatings for fibers used in the production of composite structural panels.

Patricia R McDaniel↗