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At least 199 records · Page 11

The synthesis, characterization and thermal chemistry of modified norbornenyl PMR endcaps

As part of a program to further the understanding of the polymerization of Nadic-Endcapped PMR systems, a series of model Norbornenyl-Imides has been synthesized and their thermal behavior explored. Their syntheses and characterizations as well as their rearrangement and polymerization chemistry are described. Monomer isomerization at temperatures as low as 125 C and oligomer formation at somewhat higher temperatures are observed. Approximate relative rates for competing isomerization pathways are established and some information is obtained about the details of oligomer formation. The relationship of this data to current PMR systems is briefly discussed.

Sukenik, C. N.↗

Evaluation of a high temperature adhesive for fabricating graphite/PMR-15 polyimide structures

Tests are conducted to measure shear strength, shear modulus and flatwise tensile strength of the A7F (amide-imide modified LARC-13) adhesive system. An investigation is also conducted to determine the effect of geometric material parameters, and elevated temperature on the static strength of standard joints. Single-lap and double-lap composite joints, and single, double and step lap composite to metal joints are characterized. A series of advanced joints consisting of preformed adherends, adherends with scalloped edges and joints with hybrid interface plies are tested and compared to baseline single and double-lap designs.

Hill, S. G.↗

Chemical control of rate and onset temperature of nadimide polymerization

The chemistry of norbornenyl capped imide compounds (nadimides) is briefly reviewed with emphasis on the contribution of Diels-Alder reversion in controlling the rate and onset of the thermal polymerization reaction. Control of onset temperature of the cure exotherm by adjusting the concentration of maleimide is demonstrated using selected model compounds. The effects of nitrophenyl compounds as free radical retarders on nadimide reactivity are discussed. A simple copolymerization model is proposed for the overall nadimide cure reaction. An approximate numerical analysis is carried out to demonstrate the ability of the model to simulate the trends observed for both maleimide and nitrophenyl additions.

Lauver, R. W.↗

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.↗

Charge transfer complexes of certain aromatic polyimides

By electron spectroscopy it was shown that aromatic polyimides containing electron-donor residues of diamines -C6H4-X-C6H-(X=NH, NCH3, NC6H5, O, S, and CH2) form charge transfer complexes with low-molecular-weight electron acceptors. Based on the data obtained, the hypothesis was advanced that the coloration of the polyimides per se is due to the formation of charge transfer complexes between the electron-acceptor imide fragments and the electron-donor residues of the diamines.

Gordina, T. A.↗

Process optimization of a thermoplastic polyimidesulphone

The detailed characterization of an experimental thermoplastic polyimidesulfane adhesive based on 3,3 prime-diaminodiphenylsulfone and 3,3 prime,4,4 prime-benzophenone tetracarboxylic dianhydride was studied. Model compounds were also examined. Thermal cyclization of the amide-acid to the imide was studied by a variety of techniques including DSC, TGA, MS, in situ diffuse reflectance-FTIR, and flow measurement. Characterizations were continued during the processing of adhesive tapes and the fabrication, bonding, and testing of lap shear specimens. Results provide fundamental insights into the role of cure chemistry, and the effects of residual solvent and volatile produces on processing and performance. These insights and the resulting chemical models should lead to more efficient processing cycles for these and other related thermoplastic adhesive systems.

Dezern, J. F.↗

Fire- and Heat-Resistant Laminating Resins

Imide compounds containing phosphourus thermally polymerized. New maleimido- or citraconimido-end-capped monomers, have relatively low melting temperatures, polymerized at moderate temperatures to rigid bisimide resins without elimination of volatiles. Monomers dissolve in such solvents as methyl ethyl ketone, acetone, and tetrahydrofuran, suitable and perferred as "varnish solvents" for composite fabrication. Low melting points of these componds allow use as adhesives without addition of solvents.

Kourtides, Demetrius A.↗

Processable Polyimides Containing ATBN Elastomers

Void-free moldings obtained without serious sacrifice in other properties. New synthesis produces high-temperture linear aromatic polyimide processed in imide form to yield tough, void-free components without serious sacrifice in other properties. Linear aromatic condensation polyimides are materials of prime choice for use as adhesives, composite matrix resins, films, coatings, and/or moldings where durability at temperatures as high as 200 to 300oC needed. Finding increasing use in aircraft and spacecraft applications.

St. Clair, Anne K.↗

Acetylene-Terminated Polyimide Siloxanes

Siloxane-containing addition polyimides yield toughened high-temperature adhesives and matrix resins. Addition polyimide made by reaction of aromatic tetracarboxylic acid dianhydride with aromatic diamine in presence of ethynyl-substituted aromatic monoamine. Acetylene-terminated siloxane imide cured by heating to yield acetylene-terminated polyimide siloxane.

St. Clair, Terry L.↗

Environmentally stable polymers and coatings for space application: CH-5, supplement 10

High molecular weight, randomly coupled poly(imide siloxane) soluble block copolymers were synthesized from bis(amino propyl) polydimethylsiloxane equilibrates of various molecular weights, aromatic metalinked diamines, and 3,3'-4,4'-benzophenone tetracarboxylic dianhydride (BTDA). Two synthetic procedures were successfully used to synthesize the poly(amic acid siloxane) intermediates. For both synthetic procedures, a cosolvent system was employed to achieve complete solvation of all components throughout the polymerization. Physical property characterization is continuing.

Sykes, G.↗

Soluble aromatic polyimides for film and coating applications

Linear all-aromatic polyimides have been synthesized and characterized which show much potential as films and coatings for electronic applications. Structure-property relations with regard to methods for obtaining solubility of fully imidized polymers will be discussed. Methods used to obtain solubility include variation of polymer molecular structure, variation of isomerism of the diamine monomer, modification of cure time/temperature and atmosphere. Other properties of soluble polyimides will be presented which include glass transition temperatures, thermooxidative stabilities, UV-visible spectra, and refractive indices.

St.clair, Anne K.↗

Characterization of crystalline LARC-TPI powder

LARC-TPI, a linear aromatic polyimide, developed by NASA Langley Research Center in the late 1970's had thermoplastic character, but its melt-flow properties were much lower than those of conventional thermoplastics. An imidized version of the LARC-TPI molding powder was submitted to NASA-Langley for evaluation. The initial broad melt of this material occurs in the 270 C range and reorders to higher melting forms, depending on the physical and thermal treatments. Rheological characterization of this polymer shows it to have a very low melt viscosity, which increases as the melted specie transforms to other crystalline forms with higher melting temperatures.

Burks, Harold D.↗

A DSC study on crystalline LaRC TPI powder - A new version with higher initial molecular weight

A new version of crystalline Langley Research Center Thermoplastic Polyimide (LaRC-TPI) imidized powder, which possesses a higher initial molecular weight (MW), has been prepared and characterized. The scheme used for cyclodehydration during the synthesis of this material is described. Evidence of a higher initial MW for the subject LaRC-TPI is supported by both measurements of the inherent viscosity and the DSC thermograms. An initial melting peak at 295 C is noted in the freshly-synthesized sample. The powder can be recrystallized at any elevated temperatures below 340 C, and a single crystalline endothemic peak is always observed after various thermal histories. The heat of fusion for the fresh sample, as represented by the area under the melting peak in the directional scanning calorimeter thermogram, is about 3.9 cal/gm. Comparisons of thermal properties for the subject material are made to those exhibited by the commercial LaRC-TPI powder.

Hou, Tan-Hung↗

Dry PMR-15 Resin Powders

Shelf lives of PMR-15 polymides lengthened. Procedure involves quenching of monomer reactions by vacuum drying of PRM-15 resin solutions at 70 to 90 degree F immediately after preparation of solutions. Absence of solvent eliminates formation of higher esters and reduces formation of imides to negligible level. Provides fully-formulated dry PMR-15 resin powder readily dissolvable in solvent at room temperature immediately before use. Resins used in variety of aerospace, aeronautical, and commercial applications.

Vannucci, Raymond D.↗

Developing Crystallinity In Linear Aromatic Polyimides

New technique improves melt flow of polyimide. Uses chemical imidization or cyclodehydration techniques that do not cause significant decrease in molecular weight. Process involves dissolution of polyamide acid in amide solvent or mixture of ether and amide solvent at low percentage of solids followed by treatment of this solution with aprotic organic base, such as triethylamine or pyridine, for period of time prior to treatment with organic dehydrating agent. Latter treatments facilitates formation of polyimide. Useful for production of polyimide molding materials. Expected to have widespread application in preparation of easily processed adhesives, molding powders, and matrix resins.

St. Clair, Terry L.↗

Hermetically sealable package for hybrid solid-state electronic devices and the like

A light-weight, inexpensively fabricated, hermetically sealable, repairable package for small electronic or electromechanical units, having multiple connections, is described. A molded ring frame of polyamide-imide plastic (Torlon) is attached along one edge to a base plate formed of a highly heat conducting material, such as aluminum or copper. Bores are placed through a base plate within the area of the edge surface of ring frame which result in an attachment of the ring frame to the base plate during molding. Electrical leads are molded into the ring frame. The leads are L-shaped gold-plated copper wires imbedded within widened portions of the side wall of the ring frame. Within the plastic ring frame wall the leads are bent (typically, though not necessarily at 90 deg) so that they project into the interior volume of the ring frame for connection to the solid state devices.

Miller, Wilson N.↗

Structure property behavior of polyimide siloxane segmented copolymers

Procedures were developed for preparing soluble fully imidized polyimide-polydimethyl siloxane segmented copolymers of wide ranging compositions. At low siloxane levels, the materails behave as modified polyimides. At higher concentrations, the materials are analogous to thermoplastic elastomers. Characterization by dynamic mechanical and thermal analysis methods will be reported along with an assesment of the bulk mechanical properties and the surface behavior. The surface behavior is particularly interesting since the materials can be tailored to have siloxane surfaces even at rather low siloxane contents. This influences a number of properties such as the coefficient of friction and, importanly, the degradation of these materials under aggressive oxygen environments (e.g., atomic oxygen, oxygen plasma).

Arnold, C. A.↗

Polyimide processing additives

A method has been found for enhancing the melt flow of thermoplastic polyimides during processing. A high molecular weight 422 copoly(amic acid) or copolyimide was fused with approximately 0.05 to 5 pct by weight of a low molecular weight amic acid or imide additive, and this melt was studied by capillary rheometry. Excellent flow and improved composite properties on graphite resulted from the addition of a PMDA-aniline additive to LARC-TPI. Solution viscosity studies imply that amic acid additives temporarily lower molecular weight and, hence, enlarge the processing window. Thus, compositions containing the additive have a lower melt viscosity for a longer time than those unmodified.

Pratt, J. R.↗