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At least 109 records · Page 6

An improved processible acetylene-terminated polyimide for composites

The newest member of a family of thermosetting acetylene-substituted polyimide oligomers is HR600P. This oligomer is the isoimide version of the oligomer known as HR600P and Thermid 600. Although both types of material yield the same heat resistant end products after cure, HR600P has much superior processing characteristics. This attributed to its lower melting temperature (160 + or - 10 C, 320 + or - 20 F) in contrast to 202 C (396 F) for Thermid MC-600, its longer gel time at its processing temperature (16 to 30 minutes bvs 3 minutes), and its excellent solubility in low boiling solvents such as tetrahydrofuran, glymes, or 4:1 methyl ethyl ketone/toluene mixtures. These advantages provide more acceptable coating and impregnation procedures, allow for more complete removal at lower temperatures, provide a longer pot life or working time, and allow composite structure fabrication in conventional autoclaves used for epoxy composite curing. The excellent processing characteristics of HR600P allow its use in large area laminated structures, structural composites, and molding compositions.

Landis, A. L.↗

Effects of moisture in infrared thermography of resin matrix composites

Several multiply graphite polyimide composite specimens were examined by real-time infrared thermography in order to study the effects of moisture on their thermograms. Heat was injected from one side and IR emission detected on the opposite side using AGA Thermovision System-680. No differences between the thermograms of dry and water containing specimens were detected for defect-free specimens. However, the presence of trapped water in defective specimens modified the thermographic contrast significantly. It is concluded that: (1) IR thermography can be used to detect moisture in defective composites, and (2) because of the possibility of moisture camouflaging defects, IR thermography for subsurface defect detection should be supplemented by other techniques - such as acoustical imaging and X-radiography.

Singh, J. J.↗

Low pressure process for continuous fiber reinforced polyamic acid resin matrix composite laminates

A low pressure processor was developed for preparing a well-consolidated polyimide composite laminate. Prepreg plies were formed from unidirectional fibers and a polyamic acid resin solution. Molding stops were placed at the sides of a matched metal die mold. The prepreg plies were cut shorter than the length of the mold in the in-plane lateral direction and were stacked between the molding stops to a height which was higher than the molding stops. The plies were then compressed to the height of the stops and heated to allow the volatiles to escape and to start the imidization reaction. After removing the stops from the mold, the heat was increased and 0 - 500 psi was applied to complete the imidization reaction. The heat and pressure were further increased to form a consolidated polyimide composite laminate.

Druyun, Darleen A.↗

Polyimide-Clay Composite Materials for Space Application

The introduction of nanometer-sized clay particles into a polyimide matrix has been shown to enhance the physical properties of specific polymer systems. The clay comprises large stacked platelets of the oxides of aluminum and silicon. These sheets have long dimensions on the order of tenths of a micrometer and thicknesses of several nanometers. Homogeneous dispersion of the clay platelets in the polymer matrix is necessary to achieve those enhancements in polymer properties. Natural montmorillonite with the empirical formula Na0.33Mg0.33Al1.67(OH)2(Si4O10) contains exchangeable inorganic cations. The clay lamellae stack together with the positive sodium ions situated between the surfaces of the individual sheets to balance negatively charged oxygen atoms that are on the surfaces of the sheets. These surface charges contribute to strong electrostatic forces which hold the sheets together tightly. Exfoliation can be accomplished only with unusual measures. In preparing clay nanocomposites, we have taken two steps to try to reduce these interlamellar forces in order to promote the separation (exfoliation) of the sheets and the dispersion of the individual clay particles throughout the organic polymer matrix. In the first step, some of the surface Na(+) ions are replaced with Li(+) ions. Unlike sodium cations, the lithium cations migrate into the interior of the lamellae when the system is heated. Their departure from the surface reduces the surface charge and therefore the attractive forces between the sheets. The loss of alkali metal cations from the surface can be measured as the cation exchange capacity (CEC) of the clay. For example, we found that the CEC of montmorillonite clay was reduced by almost two thirds by treating it with lithium ions and heating to 250 C for 24 hr. Lesser heating has a smaller effect on the CEC. X-ray diffraction measurements show that the d-spacing decreased from ca. 1.34 to 0.97 nm, apparently a consequence of a collapse of the clay layers. We observed that the d-spacing can be varied by altering the heat treatment. In the second part of our effort to reduce the interlamellar forces, the remaining inorganic surface cations were replaced by the trimethylphenylammonium ion (TMPA), the biphenyltrimethylammonium ion (BTMA), or the tetraphenylphosphonium ion (TPP).

Orwoll, Robert A.↗

Industry technology assessment of graphite-polymide composite materials

An assessment of the current state of the art and the future prospects for graphite polyimide composite material technology is presented. Presentations and discussions given at a minisymposium of major issues on the present and future use, availability, processing, manufacturing, and testing of graphite polyimide composite materials are summarized.

Source record↗

High Temperature VARTM with LaRC Polyimides

Recent work at NASA Langley Research Center (LaRC) has concentrated on developing new polyimide resin systems for advanced aerospace applications that can be processed without the use of an autoclave. Polyimide composites are very attractive for applications that require a high strength to weight ratio and thermal stability. Vacuum assisted resin transfer molding (VARTM) has shown potential to reduce the manufacturing cost of composite structures. In VARTM, the fibrous preform is infiltrated on a rigid tool surface contained beneath a flexible vacuum bag. Both resin injection and fiber compaction are achieved under pressures of 101.3 KPa or less. Recent studies have demonstrated the feasibility of the VARTM process for fabrication of void free structures utilizing epoxy resin systems with fiber volume fractions approaching 60%. In this work, the VARTM process has been extended to the fabrication of composite panels from polyimide systems developed at the Langley Research Center. This work has focused on processing LARC(trademark) PETI-8 (Langley Research Center Phenylethynyl Terminated Imide- 8), an aromatic polyimide based on 3,3',4,4' -biphenyltetracarboxylic dianhydride, a 50:50 molar ratio of 3,4'-oxydianiline and 1,3-bis(3-aminophenoxy)benzene, with 4-phenylethynylphthalic anhydride as the endcapping agent. Various molecular weight versions were investigated to determine their feasibility of being processed by VARTM at elevated temperatures. An injection temperature of approximately 280 C was required to achieve the necessary viscosity (<5 Poise) for flow at VARTM pressures. Laminate quality and initial mechanical properties are presented for LARC(trademark) PETI-8 and 6k IM7 uniweave fabric.

Cano, Roberto J.↗

Effects of Fiber Reinforcement Architecture on the Hygrothermal-Mechanical Performance of Polyimide Matrix Composites for Aeropropulsion Applications

A lightweight sandwich support structure, for the combustor chamber of a new generation liquid propellant rocket engine, was designed and fabricated using a polymer matrix composite (PMC) facesheet on a Ti honeycomb core. The PMC facesheet consisted of high stiffness carbon fiber, M40JB, and high temperature Polyimides, such as PMR-II-50 and HFPE-II-52. Six different fiber architectures; four harness satin (4HS) woven fabric, uni-tape, woven-uni hybrid, stitched woven fabric, stitched uni-tape and triaxial braided structures have been investigated for optimum stiffness-thickness-weight-hygrothermal performance design criteria for the hygrothermal-mechanical propulsion service exposure conditions including rapid heating up to 200 F/sec, maximum operating temperature of 600 F, internal pressure up to 100 psi. One of the specific objectives in this study is to improve composite blistering resistance in z-direction at minimum expense of in-plane mechanical properties. An extensive property-performance database including dry-wet mechanical properties at various temperatures, thermal-physical properties, such as blistering onset condition was generated for fiber architecture down-selection and design guidelines. Various optimized process methods such as vacuum bag compression molding, solvent assistant resin transfer molding (SaRTM), resin film infusion (RFI) and autoclaving were utilized for PMC panel fabrication depending on the architecture type. In the case of stitched woven fabric architecture, the stitch pattern in terms of stitch density and yarn size was optimized based on both in-plane mechanical properties and blistering performance. Potential reduction of the in-plane properties transverse to the line of stitching was also evaluated. Efforts have been made to correlate the experimental results with theoretical micro-mechanics predictions. Changes in deformation mechanism and failure sequences in terms of fiber architecture will be discussed.

Shin, E. Eugene↗

Polyimide resin composites via in situ polymerization of monomeric reactants

Thermo-oxidatively stable polyimide/graphite-fiber composites were prepared using a unique in situ polymerization of monomeric reactants directly on reinforcing fibers. This was accomplished by using an aromatic diamine and two ester-acids in a methyl alcohol solvent, rather than a previously synthesized prepolymer varnish, as with other A-type polyimides. A die molding procedure was developed and a composite property characterization conducted with high modulus graphite fiber tow. Flexure, tensile, compressive, and shear tests were conducted at temperatures from 72 to 650 F on laminates before and after exposures at the given temperatures in an air environment for times up to 1000 hours. The composite material was determined to be oxidatively, thermally, and hydrolytically stable.

Cavano, P. J.↗

Helping Aircraft Engines Lighten Up

High-temperature polyimide/carbon fiber matrix composites are developed by the Polymers Branch at NASA's Glenn Research Center. These materials can withstand high temperatures and have good processing properties, which make them particularly useful for jet and rocket engines and for components such as fan blades, bushings, and duct segments. Applying polyimide composites as components for aerospace structures can lead to substantial vehicle weight reductions. A typical polyimide composite is made up of layers of carbon or glass fibers glued together by a high-temperature polymer to make the material strong, stiff, and lightweight. Organic molecules containing carbon, nitrogen, oxygen, and hydrogen within the polyimide keep the material s density low, resulting in the light weight. The strength of a component or part made from a polyimide comes mainly from the reinforcing high-strength fibers. The strength of the carbon fibers coupled with the stiffness of polyimides allows engineers to make a very rigid structure without it being massive. Another benefit of a polyimide s suitability for aerospace applications is its reduced need for machining. When polyimide parts are removed from a mold, they are nearly in their final shape. Usually, very little machining is needed before a part is ready for use.

Source record↗

Low-Cost Resin Transfer Molding Process Developed for High-Temperature Polyimide Matrix Composites

The use of high-temperature polymer matrix composites (PMC's) in aircraft engine applications can significantly reduce engine weight and improve performance and fuel efficiency. High-temperature PMC's, such as those based on the PMR-15 polyimide matrix resin developed by the NASA Lewis Research Center, have been used extensively in military applications where performance improvements have justified their use regardless of the cost involved in producing the component. However, in commercial engines cost is a primary driver, and PMC components must be produced at costs comparable to those of the metal components that they will replace.

Source record↗

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.↗

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.↗

Kevlar/PMR-15 polyimide matrix composite for a complex shaped DC-9 drag reduction fairing

The Aircraft Energy Efficiency (ACEE) Program was established by NASA to improve the fuel efficiency of commercial transport aircraft and thereby to reduce the amount of fuel consumed by the air transportation industry. One of the final items developed by the program is an improved fairing which is the aft closure for the thrust reverser actuators on the JT8D nacelles on DC-9 aircraft. The reduced-drag fairing uses, in the interest of weight savings, an advanced composite construction. The composite material contains Kevlar 49 fibers in a PMR-15 matrix. Attention is given to the aerodynamic configuration, the material system, and aspects of fabrication development.

Kawai, R. T.↗

RTM370 Polyimide Braided Composites: Characterization and Impact Testing

RTM370 imide oligomer based on 2,3,3',4'-biphenyl dianhydride (a-BPDA), 3,4'-oxydianiline (3,4'-ODA) and terminated with the 4-phenylethynylphthalic (PEPA) endcap has been shown to exhibit a low melt viscosity (10-30 poise) at 280 C with a pot-life of 1-2 h and a high cured glass transition temperature (Tg) of 370 C. RTM370 resin has been successfully fabricated into composites reinforced with T650-35 carbon fabrics by resin transfer molding (RTM). RTM370 composites display excellent mechanical properties up to 327 C (620 F), and outstanding property retention after aging at 288degC (550 F) for 1000 h, and under hot-wet conditions. In ballistic impact testing, RTM370 triaxial braided T650-35 carbon fiber composites exhibited enhanced energy absorption at 288 C (550 F) compared to ambient temperature.

Chuang, Kathy C.↗

Polyimides formulated from a partially fluorinated diamine for aerospace tribological applications

Preliminary tribological studies on polyimides formulated from the diamine 2,2-bis 4-(4-aminophenoxy)phenyl hexafluorapane (4-BDAF) indicate that polyimides formulated from this diamine have excellent potential for high temperature tribological applications. The dianhydrides used to make the polyimides were pyromellitic (PMDA) and benzophenonetetracarboxylic acid (BTDA). Friction and wear studies at 25 and 200 C indicate that polyimides formulated using 50 mole percent of the PMDA dianhydride and 50 mole percent of the BTDA dianhydride perform better than polyimides formulated solely with the BTDA dianhydride. Graphite fiber reinforced polyimide composites were formulated with the polyimide made from the BTDA dianhydride, both graphitic and non-graphitic fibers were evaluated. Graphitic fibers produced better tribological results, since thin, flowing, "layer-like' transfer films were produced which did not build-up with long sliding durations. Non-graphitic fibers did not produce this type of transfer.

Fusaro, R. L.↗

Polyimides formulated from a partially fluorinated diamine for aerospace tribological applications

Preliminary pribological studies on polyimides formulated from the diamine 2,2-bis 4-(4-aminophenoxy)phenyl hexafluoropane (4-BDAF) indicate that polyimides formulated from this diamine have excellent potential for high temperature tribological applications. The dianhydrides used to make the polyimides were pyromellitic (PMDA) and benzophenonetetracarboxylic acid (BTDA). Friction and wear studies at 25 and 200 C indicate that polyimides formulated using 50 mole percent of the PMDA dianhydride and 50 mole percent of the BTDA dianhydride perform better than polyimides formulated solely with the BTDA dianhydride. Graphite fiber reinforced polyimide composites were formulated with the polyimide made from the BTDA dianhydride and both graphitic and non-graphitic fibers were evaluated. Graphitic fibers produced better tribological results, since thin, flowing, 'layer-like' transfer films were produced which did not build up with long sliding durations. Non-graphitic fibers did not produce this type of transfer. Previously announced in STAR as N83-22423

Fusaro, R. L.↗

Interlaminar fracture toughness of thermoplastic composites

Edge delamination tension and double cantilever beam tests were used to characterize the interlaminar fracture toughness of continuous graphite-fiber composites made from experimental thermoplastic polyimides and a model thermoplastic. Residual thermal stresses, known to be significant in materials processed at high temperatures, were included in the edge delamination calculations. In the model thermoplastic system (polycarbonate matrix), surface properties of the graphite fiber were shown to be significant. Critical strain energy release rates for two different fibers having similar nominal tensile properties differed by 30 to 60 percent. The reason for the difference is not clear. Interlaminar toughness values for the thermoplastic polyimide composites (LARC-TPI and polyimidesulfone) were 3 to 4 in-lb/sq in. Scanning electron micrographs of the EDT fracture surfaces suggest poor fiber/matrix bonding. Residual thermal stresses account for up to 32 percent of the strain energy release in composites made from these high-temperature resins.

Hinkley, J. A.↗

Interlaminar fracture toughness of thermoplastic composites

Edge delamination tension and double cantilever beam tests were used to characterize the interlaminar fracture toughness of continuous graphite-fiber composites made from experimental thermoplastic polyimides and a model thermoplastic. Residual thermal stresses, known to be significant in materials processed at high temperatures, were included in the edge delamination calculations. In the model thermoplastic system (polycarbonate matrix), surface properties of the graphite fiber were shown to be significant. Cricital strain energy release rates for two different fibers having similar nominal tensile properties differed by 30 to 60 percent. The reason for the difference is not clear. Interlaminar toughness values for the thermoplastic polyimide composites (LARC-TPI and polyimidesulfone) were 3 to 4 in-lb/sq in. Scanning electron micrographs of the EDT fracture surfaces suggest poor fiber/matrix bonding. Residual thermal stresses account for up to 32 percent of the strain energy release in composites made from these high-temperature resins.

Hinkley, Jeffrey A.↗