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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records

Correlations of norbornenyl crosslinked polyimide resin structures with resin thermo-oxidative stability, resin glass transition temperature and composite initial mechanical properties

PMR (polymerization of monomeric reactants) methodology was used to prepare 70 different polyimide oligomeric resins and 30 different unidirectional graphite fiber/polyimide composites. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on resin thermo-oxidative stability and glass transition temperature (Tg) of the cured/postcured resins. A linear correlation of decreasing 316 C resin weight loss/surface area versus (1) decreasing aliphatic content, or (2) increasing benzylic/aliphatic content stoichiometry ratio over a wide range of resin compositions was observed. An almost linear correlation of Tg versus molecular distance between the crosslinks was also observed. An attempt was made to correlate Tg with initial composite mechanical properties (flexural strength and interlaminar shear strength). However, the scatter in mechanical strength data prevented obtaining a clear correlation. Instead, only a range of composite mechanical properties was obtained at 25, 288, and 316 C. Perhaps more importantly, what did become apparent during the correlation study was (1) the PMR methodology could be used to prepare composites from resins containing a wide variety of monomer modifications, (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins formulated exhibited satisfactory processing flow, and (3) that PMR resins exhibited predictable rates of 316 C weight loss/surface area based on their benzylic/aliphatic stoichiometery ratio.

Alston, William B.

Resin impregnation process for producing a resin-fiber composite

Process for vacuum impregnation of a dry fiber reinforcement with a curable resin to produce a resin-fiber composite, by drawing a vacuum to permit flow of curable liquid resin into and through a fiber reinforcement to impregnate same and curing the resin-impregnated fiber reinforcement at a sufficient temperature and pressure to effect final curing. Both vacuum and positive pressure, e.g. autoclave pressure, are applied to the dry fiber reinforcement prior to application of heat and prior to any resin flow to compact the dry fiber reinforcement, and produce a resin-fiber composite of reduced weight, thickness and resin content, and improved mechanical properties. Preferably both a vacuum and positive pressure, e.g. autoclave pressure, are also applied during final curing.

Palmer, Raymond J.

Low Melt Viscosity Resins for Resin Transfer Molding

In recent years, resin transfer molding (RTM) has become one of the methods of choice for high performance composites. Its cost effectiveness and ease of fabrication are major advantages of RTM. RTM process usually requires resins with very low melt viscosity (less than 10 Poise). The optimum RTM resins also need to display high thennal-oxidative stability, high glass transition temperature (T(sub g)), and good toughness. The traditional PMR-type polyimides (e.g. PMR-15) do not fit this requirement, because the viscosities are too high and the nadic endcap cures too fast. High T(sub g), low-melt viscosity resins are highly desirable for aerospace applications and NASA s Reusable Launch Vehicle (RLV) program. The objective of this work is to prepare low-melt viscosity polyimide resins for RTM or resin film infusion (RFI) processes. The approach involves the synthesis of phenylethynyl-terminated imide oligomers. These materials have been designed to minimize their melt viscosity so that they can be readily processed. During the cure, the oligomers undergo both chain extension and crosslinking via the thermal polymerization of the phenylethynyl groups. The Phenylethynyl endcap is preferred over the nadic group due to its high curing temperature, which provides broader processing windows. This work involved the synthesis and polymerization of oligomers containing zig-zag backbones and twisted biphenyl structures. Some A-B type precursors which possessed both nitro and anhydride functionality, or both nitro and amine functionality, were also synthesized in order to obtain the well defined oligomers. The resulting zig-zag structured oligomers were then end-capped with 4-phenylethynylphthalic anhydride (PEPA) for further cure. The properties of these novel imide oligomers are evaluated.

Harris, Frank W.

Foam, Foam-resin composite and method of making a foam-resin composite

This invention relates to a foam, a foam-resin composite and a method of making foam-resin composites. The foam set forth in this invention comprises a urethane modified polyisocyanurate derived from an aromatic amino polyol and a polyether polyol. In addition to the polyisocyanurate foam, the composite of this invention further contains a resin layer, wherein the resin may be epoxy, bismaleimide, or phenolic resin. Such resins generally require cure or post-cure temperatures of at least 350.degree. F.

Cranston, John A.

Structure-to-property Relationships in Addition Cured Polymers 2: Resin Tg Composite Initial Mechanical Properties of Norbornenyl Cured Polyimide Resins

PRM (polymerization of monomeric reactants) methodology was used to prepare thirty different polyimide oligomeric resins. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on glass transition temperature (Tg) of the cured/postcured resins. An almost linear correlation of Tg versus molecular distance between the crosslinks was observed. An attempt was made to correlate Tg with initial mechanical properties (flexural strength and interlaminar shear strength) of unidirectional graphite fiber composites prepared with these resins. However, the scatter in mechanical strength data prevented obtaining as clear a correlation as was observed for the structural modification/crosslink distance versus Tg. Instead, only a range of composite mechanical properties was obtained at the test temperatures studied (room temperature, 288 and 316 C). Perhaps more importantly, what did become apparent during the attempted correlation study was: (1) that PMR methodology could be used to prepare composites from resins that contain a wide variety of monomer modifications, and (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins selected were melt processable.

Alston, W. B.

Structure-to-property relationships in addition cured polymers. II - Resin Tg and composite initial mechanical properties of norbornenyl cured polyimide resins

PRM (polymerization of monomeric reactants) methodology was used to prepare thirty different polyimide oligomeric resins. Monomeric composition as well as chain length between sites of crosslinks were varied to examine their effects on glass transition temperature (Tg) of the cured/postcured resins. An almost linear correlation of Tg versus molecular distance between the crosslinks was observed. An attempt was made to correlate Tg with initial mechanical properties (flexural strength and interlaminar shear strength) of unidirectional graphite fiber composites prepared with these resins. However, the scatter in mechanical strength data prevented obtaining as clear a correlation as was observed for the structural modification/crosslink distance versus Tg. Instead, only a range of composite mechanical properties was obtained at the test temperatures studied (room temperature, 288 and 316 C). Perhaps more importantly, what did become apparent during the attempted correlation study was: (1) that PMR methodology could be used to prepare composites from resins that contain a wide variety of monomer modifications, and (2) that these composites almost invariably provided satisfactory initial mechanical properties as long as the resins selected were melt processable.

Alston, William B.

Phenoxy resins containing pendent ethynyl groups and cured resins obtained therefrom

Phenoxy resins containing pendent ethynyl groups, the process for preparing the same, and the cured resin products obtained therefrom are disclosed. Upon the application of heat, the ethynyl groups react to provide branching and crosslinking with the cure temperature being lowered by using a catalyst if desired but not required. The cured phenoxy resins containing pendent ethynyl groups have improved solvent resistance and higher use temperature than linear uncrosslinked phenoxy resins and are applicable for use as coatings, films, adhesives, composited matrices and molding compounds.

Hergenrother, P. M.

Development of resins for composites by resin transfer molding

Designed to cover a wide range of resin technology and to meet the near-term and long-term needs of the aircraft industry, this research has three objectives: to produce resin transfer molding (RES) resins with improved processability, to produce prepreg systems with high toughness and service temperature, and to produce new resin systems. Progress on reaching the objectives is reported.

Woo, Edmund P.

Low-melt Viscosity Polyimide Resins for Resin Transfer Molding (RTM) II

A series of polyimide resins with low-melt viscosities in the range of 10-30 poise and high glass transition temperatures (Tg s) of 330-370 C were developed for resin transfer molding (RTM) applications. These polyimide resins were formulated from 2,3,3 ,4 -biphenyltetracarboxylic dianhydride (a-BPDA) with 4-phenylethynylphthalic anhydride endcaps along with either 3,4 - oxyaniline (3,4 -ODA), 3,4 -methylenedianiline, (3,4 -MDA) or 3,3 -methylenedianiline (3,3 -MDA). These polyimides had pot lives of 30-60 minutes at 260-280 C, enabling the successful fabrication of T650-35 carbon fiber reinforced composites via RTM process. The viscosity profiles of the polyimide resins and the mechanical properties of the polyimide carbon fiber composites will be discussed.

Chuang, Kathy C.

Comparison of resin film infusion, resin transfer molding, and consolidation of textile preforms for primary aircraft structure

Innovative design concepts and cost effective fabrication processes were developed for damage tolerant primary structures that can perform at a design ultimate strain level of 6000 micro inch/inch. Attention focused on the use of textile high performance fiber reinforcement concepts that provide improved damage tolerance and out-of-plane load capability, low cost resin film infusion (RFI) and resin transfer molding (RTM) processes, and thermoplastic forming concepts. The fabrication of wing 'Y' spars by four different materials and/or processes methods is described: fabricated using IM7 angle interlock 0 to 90 deg woven preforms with + or - 45 deg plies stitched with Toray high strength graphite thread and processed using RFI and 3501-6 epoxy; fabricated using G40-800 knitted/stitched preforms and processed using RFI and 3501-6 epoxy; fabricated using G40-800 knitted/stitched preforms using RTM and Tactix 123/H41 epoxy; and fabricated preforms using AS4(6K)/PEEK 150 g commingled angle interlock 0 to 90 deg woven preforms with + or - 45 deg commingled plies stitched using high strength graphite thread and processed by consolidation. Structural efficiency, processability, and acquisition cost are compared.

Suarez, J.

Comparison of resin film infusion, resin transfer molding, and consolidation of textile preforms for primary aircraft structure

Under NASA's Novel Composites for Wing and Fuselage Applications (NCWFA) Program, Grumman is developing innovative design concepts and cost-effective fabrication processes for damage-tolerant primary structures that can perform at a design ultimate strain level of 6000 micro-inch/inch. Attention has focused on the use of textile high-performance fiber-reinforcement concepts that provide improved damage tolerance and out-of-plane load capability, low-cost resin film infusion (RFI) and resin transfer molding (RTM) processes, and thermoplastic forming concepts. The fabrication of wing 'Y' spars by four different materials/processes methods is described: 'Y' spars fabricated using IM7 angle interlock 0/90 deg woven preforms with +/- 45 deg plies stitched with Toray high-strength graphite thread and processed using RFI and 3501-6 epoxy; 'Y' spars fabricated using G40-800 knitted/stitched preforms and processed using RFI and 3501-6 epoxy; 'Y' spars fabricated using G40-800 knitted/stitched preforms and processed using RTM and Tactix 123/H41 epoxy; and 'Y' spars fabricated using AS4(6k)/PEEK 150-g commingled angle interlock 0/90 deg woven preforms with +/- 45 deg commingled plies stitched using high-strength graphite thread and processed by consolidation. A comparison of the structural efficiency, processability, and projected acquisition cost of these representative spars is presented.

Suarez, J.

Impact properties of rubber-modified epoxy resin-graphite-fiber composites

To improve the impact resistance of graphite-fiber composites, a commercial and an experimental epoxy resin were modified with liquid reactive rubber and a brominated epoxy resin. The commercial epoxy was a tetrafunctional resin, and the experimental epoxy was a trifunctional resin. The reactive rubber was a carboxyl-terminated butadiene-acrylonitrile copolymer. The rubber content was varied from 0 to 25 percent (wt). The brominated epoxy resin was used at Br levels of 4, 19, and 35 percent of the resin. Composites were prepared with woven graphite cloth reinforcement. The composites were evaluated by using flexural strength in the dry state and an elevated temperature after saturation with water. The impact properties were determined by measuring shear strength after falling-ball impact and instrumented impact. The rubber-modified, trifunctional resin exhibited better properties, when tested in hot-wet conditions in a heated oven at 366 K (after boiling the material for 2 h in demineralized water), than the tetrafunctional resin. Improved impact resistance was observed with the addition of the reactive rubber to the epoxy resin. Further improvement was observed with the addition of the brominated epoxy resin.

Gilwee, W. J.

Low Density Resin Impregnated Ceramic Article Having an Average Density of 0.15 to 0.40 G/CC

A low-density resin impregnated ceramic article advantageously employed as a structural ceramic ablator comprising a fired preform of ceramic fibers. The fibers of the ceramic preform are coated with an organic resin film. The organic resin can be a thermoplastic resin or a cured thermosetting resin. In one embodiment, the resin is uniformly distributed within the ceramic article. In a second embodiment, the resin is distributed so as to provide a density gradient along at least one direction of the ceramic article. The resin impregnated ceramic article is prepared by providing a fired preform of ceramic fibers; immersing the preform of ceramic fibers in a solution of a solvent and an organic resin infiltrant; and removing the solvent to form a resin film on the ceramic fibers.

Tran, Huy K.

Low-density resin impregnated ceramic article and method for making the same

A low-density resin impregnated ceramic article advantageously employed as a structural ceramic ablator comprising a matrix of ceramic fibers. The fibers of the ceramic matrix are coated with an organic resin film. The organic resin can be a thermoplastic resin or a cured thermosetting resin. In one embodiment, the resin is uniformly distributed within the ceramic article. In a second embodiment, the resin is distributed so as to provide a density gradient along at least one direction of the ceramic article. The resin impregnated ceramic article is prepared by providing a matrix of ceramic fibers; immersing the matrix of ceramic fibers in a solution of a solvent and an organic resin infiltrant; and removing the solvent to form a resin film on the ceramic fibers.

Tran, Huy K.

Composites with improved fiber-resin interfacial adhesion

The adhesion of fiber reinforcement such as high modulus graphite to a matrix resin such as polycarbonate is greatly enhanced by applying a very thin layer, suitably from 50 Angstroms to below 1000 Angstroms, to the surface of the fiber such as by immersing the fiber in a dilute solution of the matrix resin in a volatile solvent followed by draining to remove excess solution and air drying to remove the solvent. The thin layer wets the fiber surface. The very dilute solution of matrix resin is able to impregnate multifilament fibers and the solution evenly flows onto the surface of the fibers. A thin uniform layer is formed on the surface of the fiber after removal of the solvent. The matrix resin coated fiber is completely wetted by the matrix resin during formation of the composite. Increased adhesion of the resin to the fibers is observed at fracture. At least 65 percent of the surface of the graphite fiber is covered with polycarbonate resin at fracture whereas uncoated fibers have very little matrix resin adhering to their surfaces at fracture and epoxy sized graphite fibers exhibit only slightly higher coverage with matrix resin at fracture. Flexural modulus of the composite containing matrix resin coated fibers is increased by 50 percent and flexural strength by 37 percent as compared to composites made with unsized fibers.

Cizmecioglu, Muzaffer

Acetylene-chromene terminated resins as high temperature thermosets

A novel phase transfer catalyzed process for the preparation of propargyl ethers has been developed. The propargyl ethers serve as precursors to a new class of thermosetting resins called acetylene-chromene terminated (ACT) resins. Heat treatment of a solution of propargyl ethers with various catalysts, followed by removal of solvent leads to the ACT resins via partial conversion of the propargyl ether groups to chromenes. This process reduces the energy content of the resin systems and reduces the amount of shrinkage found during cure. Due to the presence of the solvent the process is safe and gives rise to low viscosity products suitable for resin transfer molding and filament winding type applications. Due to the high glass transition temperature, high modulus, and low moisture uptake the cured resins display better than 232 C/wet performance. The thermal stability of the ACT resins in air at 204 C is superior to that of conventional bismaleimide resins. The resins also display excellent electrical properties.

Godschalx, J. P.