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All sourcesNASA NTRSDOE OSTI
NASA NTRS2004

Processing Robustness for A Phenylethynyl Terminated Polyimide Composite

The processability of a phenylethynyl terminated imide resin matrix (designated as PETI-5) composite is investigated. Unidirectional prepregs are made by coating an N-methylpyrrolidone solution of the amide acid oligomer (designated as PETAA-5/NMP) onto unsized IM7 fibers. Two batches of prepregs are used: one is made by NASA in-house, and the other is from an industrial source. The composite processing robustness is investigated with respect to the prepreg shelf life, the effect of B-staging conditions, and the optimal processing window. Prepreg rheology and open hole compression (OHC) strengths are found not to be affected by prolonged (i.e., up to 60 days) ambient storage. Rheological measurements indicate that the PETAA-5/NMP processability is only slightly affected over a wide range of B-stage temperatures from 250 deg C to 300 deg C. The OHC strength values are statistically indistinguishable among laminates consolidated using various B-staging conditions. An optimal processing window is established by means of the response surface methodology. IM7/PETAA-5/NMP prepreg is more sensitive to consolidation temperature than to pressure. A good consolidation is achievable at 371 deg C (700 deg F)/100 Psi, which yields an RT OHC strength of 62 Ksi. However, processability declines dramatically at temperatures below 350 deg C (662 deg F), as evidenced by the OHC strength values. The processability of the IM7/LARC(TM) PETI-5 prepreg was found to be robust.

Hou, Tan-Hung↗
NASA NTRS2009

Polyimide Composites Based on Asymmetric Dianhydrides (a-ODPA vs a-BPDA)

Two series of low-melt viscosity imide resins (2-15 poise at 260-280 C) were formulated from either asymmetric oxydiphthalic anhydride (a-ODPA) or asymmetric biphenyl dianhydride (a- BPDA) with 4-phenylethynyl endcap (PEPA), along with 3,4'-oxydianiline, 3,4 - methylenedianiline, 3,3 -methylenedianiline or 3,3 -diaminobenzophenone, using a solvent-free melt process. These low-melt viscosity imide resins were fabricated into polyimide/T650-35 carbon fabric composites by resin transfer molding (RTM). Composites from a-ODPA based resins display better open-hole compression strength and short beam shear strength from room temperature to 288 C than that of the corresponding a-BPDA based resins. However, due to the lower Tg s of a-ODPA based resins (265-330 C), their corresponding composites do not possess 315 C use capability while the a-BPDA based composites do. In essence, RTM 370 (T g = 370 C), derived from a-BPDA and 3,4 -ODA and PEPA, exhibits the best overall property performance at 315 C (600 F).

Chuang, Kathy C.↗
NASA NTRS2011

Polyimide Composites Properties of RTM370 Fabricated by Vacuum Assisted Resins Transfer Molding (VARTM)

RTM370 imide resin based on 2,3,3 ,4 -biphenyl dianhydride ( a-BPDA), 3,4 -oxydianinline (3,4 -ODA) with 4-phenylethynylphthalic (PEPA) endcap has shown to exhibit high Tg (370 C) and low melt viscosity (10-30 poise) at 280 C with a pot-life of 1-2 h. Previously, RTM370 resin has been fabricated into composites with T650-35 carbon fabrics by resin transfer molding (RTM) successfully. RTM370 composites exhibit excellent mechanical properties up to 327 C (620 F), and outstanding property retention after aging at 288 C (550 F) for 1000 hrs. In this presentation, RTM 370 composites will be fabricated by vacuum assisted resins transfer molding (VARTM), using vacuum bags without mold. The mechanical properties of RTM370 composites fabricated by VARTM will be compared to those of RTM370 made by RTM.

Chuang, Kathy C.↗
NASA NTRS2009

Polyimide Composites Based on Asymmetric Dianhydrides (a-ODPA vs a-BPDA)

RTM Resins based on a-ODPA and a-BPDA with kinked diamines exhibit low-melt viscosity (approximately 10 poise). Composites made from a-ODPA resins (T(sub g) = 265-330 C) by RTM display good mechanical properties at 288 C (550 F), but soften at 315 C (600 F). Composites of RTM370 based on a-BPDA retain excellent mechanical properties at 315 C, exceeding BMI-5270-1 capability.

Chuang, Kathy C.↗
NASA NTRS2012

Processing and Properties of Vacuum Assisted Resin Transfer Molded Phenylethynyl Terminated Imide Composites

Polyimide composites are very attractive for applications that require a high strength to weight ratio and thermal stability. Recent work at NASA Langley Research Center (LaRC) has concentrated on developing new polyimide resin systems that can be processed without the use of an autoclave for advanced aerospace applications. Due to their low melt viscosities and long melt stability, certain phenylethynyl terminated imides (PETI) can be processed into composites using high temperature vacuum assisted resin transfer molding (HT-VARTM). VARTM has shown the potential to reduce the manufacturing cost of composite structures. In the current study, two PETI resins, LARC(Trademark) PETI-330 and LARC(Trademark) PETI-9, were infused into carbon fiber preforms at 260 C and cured at temperatures up to 371 C. Photomicrographs of polished cross sections were taken and void contents, determined by acid digestion, were below 4.5%. Mechanical properties including short block compression (SBC), compression after impact (CAI), and open hole compression (OHC) were determined at room temperature, 177 C, and 288 C. Both PETI-9 and PETI-330 composites demonstrated very good retention of mechanical properties at elevated temperatures. SBC and OHC properties after aging for 1000 hours at temperatures up to 288 C were also determined.

Cano, Roberto J.↗
NASA NTRS1989

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.↗
NASA NTRS1995

A polyimide molecular composite

A polyimide is a hard and sturdy thermoplastic made from the combination of tetracarboxylic dianhydrides and diamines in a polar aprotic solvent. A series of polyimide blends comprising of a tough moldable, wholly aromatic polyimide and a highly crystalline rigid polyimide were prepared. The flexible polyimide was based on LaRC-SI with a 2% offset, and the rigid polyimide as based on para-phenylenediamine and biphenyltetracarboxylic dinnhydride encapped with pthalic anhydride. The polyimide blends were cast as films and cured at 100, 200, and 300 C in air. These films were characterized by finding their glass-transition temperature, melting temperature, coefficient of thermal expansion, tensile modulus, tensile strength, and percent elongation. These characterizations found out which polyimide blend had exceptional mechanical and thermal properties. Experimental results showed the following: (1) A blend with increasing amounts of flexible polyimide produced a better film; (2) A blend with increasing amounts of rigid polyimide produced a brittle film; (3) LaRC-SI (2% offset) tended to phase separate during film casting; (4) Most of the films produced were brittle; and (5) There was an inability to obtain mechanical and thermal properties due to having brittle film. These conclusions demonstrate the difficulty in producing a polyimide blend comprising two physically distinct polyimides. Combining a polysmide with a poly(amic acid) thermosett could be the next phase of research in polyimide synthesis.

Hart, Aprill J.↗
NASA NTRS1989

Polyimide matrix composites - Polyimidesulfone/LARC-TPI (1:1) blend

Polyimide matrix composites were fabricated from unidirectional unsized AS-4 carbon fiber and a doped 1:1 blend of two polyimides: PISO2 and LARC-TPI. To enhance melt flow properties, the molecular weight of the PISO2 was controlled by end-capping with phthalic anhydride and addition of 5 percent by weight p-phenylenediamine-phthalic anhydride bisamic acid dopant. Prepreg was drum-wound using a diglyme slurry comprised of the soluble polyamideacid of PISO2, the soluble bisamideacid of the dopant, and the insoluble imidized LARC-TPI powder. Melt flow studies with a rotary rheometer and parallel plate plastometer on neat resin and prepreg helped develop an optimum cure cycle. Composite mechanical properties at room and elevated temperatures, dry and moisture-saturated, were evaluated, including short beam shear strength and flexure, tensile, shear, and compression properties. Two 18 x 24-inch skin-stringer panels were fabricated, one of which was tested in compression to failure.

Johnston, Norman J.↗
NASA NTRS1989

Polyimide Matrix composites: Polyimidesulfone/LARC-TPI (1:1) blend

Polyimide matrix composites were fabricated from unidirectional unsized AS-4 carbon fiber and a doped 1:1 blend of two polyimides: benzophenone dianhydride-3,3'-diamino diphenylsulfone (PISO2) and benzophenone dianhydride-3,3'-diamino benzophenone (LARC-TPI). To enhance melt flow properties, the molecular weight of the PISO2 was controlled by end-capping with phthalic anhydride and addition of 5 percent by weight p-phenylene diamine-phthalic anhydride bisamic acid dopant. Prepreg was drum-wound using a diglyme slurry comprised of the soluble polyamideacid of PISO2, the soluble bisamideacid of the dopant, and the insoluble imidized LARC-TPI powder. Melt flow studies with a rotary rheometer and parallel plate plastometer on neat resin and prepreg helped develop an optimum cure cycle. Composite mechanical properties at room and elevated temperatures, dry and moisture-saturated, were evaluated, including short beam shear strength and flexure, tensile, shear, and compression properties. Two 18 in. x 24 in. skin-stringer panels were fabricated, one of which was tested in compression to failure.

Johnston, Norman J.↗
NASA NTRS2014

Polyimide Cellulose Nanocrystal Composite Aerogels

Polyimide (PI) aerogels are highly porous solids having low density, high porosity and low thermal conductivity with good mechanical properties. They are ideal for various applications including use in antenna and insulation such as inflatable decelerators used in entry, decent and landing operations. Recently, attention has been focused on stimuli responsive materials such as cellulose nano crystals (CNCs). CNCs are environmentally friendly, bio-renewable, commonly found in plants and the dermis of sea tunicates, and potentially low cost. This study is to examine the effects of CNC on the polyimide aerogels. The CNC used in this project are extracted from mantle of a sea creature called tunicates. A series of polyimide cellulose nanocrystal composite aerogels has been fabricated having 0-13 wt of CNC. Results will be discussed.

Aerogels↗
NASA NTRS1994

A manufacturing database of advanced materials used in spacecraft structures

Cost savings opportunities over the life cycle of a product are highest in the early exploratory phase when different design alternatives are evaluated not only for their performance characteristics but also their methods of fabrication which really control the ultimate manufacturing costs of the product. In the past, Design-To-Cost methodologies for spacecraft design concentrated on the sizing and weight issues more than anything else at the early so-called 'Vehicle Level' (Ref: DOD/NASA Advanced Composites Design Guide). Given the impact of manufacturing cost, the objective of this study is to identify the principal cost drivers for each materials technology and propose a quantitative approach to incorporating these cost drivers into the family of optimization tools used by the Vehicle Analysis Branch of NASA LaRC to assess various conceptual vehicle designs. The advanced materials being considered include aluminum-lithium alloys, thermoplastic graphite-polyether etherketone composites, graphite-bismaleimide composites, graphite- polyimide composites, and carbon-carbon composites. Two conventional materials are added to the study to serve as baseline materials against which the other materials are compared. These two conventional materials are aircraft aluminum alloys series 2000 and series 7000, and graphite-epoxy composites T-300/934. The following information is available in the database. For each material type, the mechanical, physical, thermal, and environmental properties are first listed. Next the principal manufacturing processes are described. Whenever possible, guidelines for optimum processing conditions for specific applications are provided. Finally, six categories of cost drivers are discussed. They include, design features affecting processing, tooling, materials, fabrication, joining/assembly, and quality assurance issues. It should be emphasized that this database is not an exhaustive database. Its primary use is to make the vehicle designer aware of some of the most important aspects of manufacturing associated with his/her choice of the structural materials. The other objective of this study is to propose a quantitative method to determine a Manufacturing Complexity Factor (MCF) for each material being contemplated. This MCF is derived on the basis of the six cost drivers mentioned above plus a Technology Readiness Factor which is very closely related to the Technology Readiness Level (TRL) as defined in the Access To Space final report. Short of any manufacturing information, our MCF is equivalent to the inverse of TRL. As more manufacturing information is available, our MCF is a better representation (than TRL) of the fabrication processes involved. The most likely application for MCF is in cost modeling for trade studies. On-going work is being pursued to expand the potential applications of MCF.

Bao, Han P.↗
NASA NTRS1972

Low void content autoclave molded titanium alloy and polyimide graphite composite structures.

This paper discusses a resin developed for use in autoclave molding of polyimide graphite composite stiffened, titanium alloy structures. Both primary and secondary bonded structures were evaluated that were produced by autoclave processing. Details of composite processing, adhesive formulary, and bonding processes are provided in this paper, together with mechanical property data for structures. These data include -65 F, room temperature, and 600 F shear strengths; strength retention after aging; and stress rupture properties at 600 F under various stress levels for up to 1000 hours duration. Typically, shear strengths in excess of 16 ksi at room temperature with over 60% strength retention at 600 F were obtained with titanium alloy substrates.

Vaughan, R. W.↗
NASA NTRS1988

A review of dynamic mechanical characterization of high temperature PMR polyimides and composites

This paper reviews the applications of dynamic mechanical characterization for high-temperature PMR polyimides and their graphite-fiber-reinforced composites. This characterization technique provides insights into the processability, performance, and structure property relationships of the polyimides and composites. The dynamic mechanical properties of various molding powders, commercially obtained prepregs, neat resins, and as-fabricated as well as aged composites are presented. Some applied aspects of the dynamic mechanical data are discussed.

Pater, Ruth H.↗
NASA NTRS1991

Squeeze flow and compaction behavior of toughened polyimide matrix composites

The main emphasis was placed upon the squeeze flow and compaction behavior of the Lewis Research Center (LaRC) research project series polyimide matrix composites. The measurement of squeeze film flow behavior was performed by a plastometer which monitors the change of thickness of a prepreg specimen laid between two parallel plates under the specified temperature and pressure history. A critical evaluation of the plastometer data was attempted by examining the morphology of the specimen at various points during the squeeze flow. The effects of crosslinks (Mc) of resin, imidization (B-ataging) condition, and pressure on the squeeze flow behavior were examined. Results are given.

Lee, Byung Lip↗
NASA NTRS1990

Microcracking mechanisms and interface toughening of semi-IPN polyimide matrix composites

A new research program was initiated as a preliminary phase. The following three objectives are being pursued for the overall program: to elucidate the mechanisms of microcracking for graphite fiber-reinforced semi-IPN polyimide matrix composites under mechanical and thermal cyclic loading; to devise material engineering solutions for possible improvement of fatigue damage resistance (or the increase of fatigue endurance strength) of semi-IPN matrix composites by tailoring of modulus and toughness of fiber-resin interface region; and to assess processing characteristics of the composites and their roles in controlling the resistance of composites to microcracking and the effectiveness of interface toughening. The main emphasis was placed upon the initial screening of material systems and optimization of processing conditions for semi-IPN matrix composites with tailored interface. As a first set of control material systems to study, the composites were prepared with unsized Celion 6000 graphite fiber reinforcement and the following resin matrices of varied fracture toughness: PMR-15 thermoset polyimide, semi-IPN of PNR-15 thermoset polyimide and NR150B2 thermoplastic polyimide in 75/25 ratio, and semi-IPN of PMR-15 and NR150B2 in 50/50 ratio. For the composites with the resin matrix of semi-IPN in 75/25 ratio, interface tailoring was attempted by using graphite fibers coated with the resins of systematically varied fracture toughness. In the continuing work, a broad range of interlayer toughness will be achieved by coating the fibers with reactants of semi-IPN having lower or higher content of thermoplastic constituent in comparison with the composition of surrounding resin matrix. In pursuing the objectives of the overall research program, the respective roles and interaction of critical parameters were defined.

Lee, Byung L.↗
NASA NTRS2000

Shelf Life of PMR Polyimide Monomer Solutions and Prepregs Extended

PMR (Polymerization of Monomeric Reactants) technology was developed in the mid-1970's at the NASA Glenn Research Center at Lewis Field for fabricating high-temperature stable polyimide composites. This technology allowed a solution of polyimide monomers or prepreg (a fiber, such as glass or graphite, impregnated with PMR polyimide monomers) to be thermally cured without the release of volatiles that cause the formation of voids unlike the non-PMR technology used for polyimide condensation type resins. The initial PMR resin introduced as PMR 15 is still commercially available and is used worldwide by aerospace industries as the state-of-the-art resin for high-temperature polyimide composite applications. PMR 15 offers easy composite processing, excellent composite mechanical property retention, a long lifetime at use temperatures of 500 to 550 F, and relatively low cost. Later, second-generation PMR resin versions, such as PMR II 50 and VCAP 75, offer improvements in the upper-use temperature (to 700 F) and in the useful life at temperature without major compromises in processing and property retention but with significant increases in resin cost. Newer versions of nontoxic (non-methylene dianiline) PMR resins, such as BAX PMR 15, offer similar advantages as originally found for PMR 15 but also with significant increases in resin cost. Thus, the current scope of the entire PMR technology available meets a wide range of aeronautical requirements for polymer composite applications.

Alston, William B.↗
NASA NTRS1979

Development and demonstration of manufacturing processes for fabricating graphite/PMR-15 polyimide structural elements

The processing requirements for graphite/PMR-15 polyimide composites developed to demonstrate the structural integrity of polyimide composite structural elements at temperatures up to 589K (600 F) are described. Major tasks included: quality assurance development; materials and process development; specification verification; flat panel fabrication; stiffened panel fabrication; honeycomb panel fabrication; chopped fiber moldings; and demonstration component fabrication. Materials, processing, and quality assurance documents were prepared from experimentally derived data. Structural elements consisting of flat panels, corrugated stiffeners, I-beams, hat stiffeners, honeycomb panels, and chopped fiber moldings were made and tested. Property data from 219K (-65 F) to 589K (600 F) were obtained. All elements were made in a production environment. The size of each element was sufficient to insure production capability and structural component applicability. Problems associated with adhesive bonding, laminate and structural element analysis, material variability, and test methods were addressed.

Sheppard, C. H.↗