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Jensen, B. J.

Publications and source records attributed to Jensen, B. J..

Evaluation of Double-Vacuum-Bag Process For Composite Fabrication

A non-autoclave vacuum bag process using atmospheric pressure alone that eliminates the need for external pressure normally supplied by an autoclave or a press is an attractive method for composite fabrication. This type of process does not require large capital expenditures for tooling and processing equipment. In the molding cycle (temperature/pressure profile) for a given composite system, the vacuum application point has to be carefully selected to achieve the final consolidated laminate net shape and resin content without excessive resin squeeze-out. The traditional single-vacuum- bag (SVB) process is best suited for molding epoxy matrix based composites because of their superior flow and the absence of reaction by-products or other volatiles. Other classes of materials, such as polyimides and phenolics, generate water during cure. In addition, these materials are commonly synthesized as oligomers using solvents to facilitate processability. Volatiles (solvents and reaction byproducts) management therefore becomes a critical issue. SVB molding, without additional pressure, normally fails to yield void-free quality composites for these classes of resin systems. A double-vacuum- bag (DVB) process for volatile management was envisioned, designed and built at the NASA Langley Research Center. This experimental DVB process affords superior volatiles management compared to the traditional SVB process. Void-free composites are consistently fabricated as measured by C-scan and optical photomicroscopy for high performance polyimide and phenolic resins.

Hou, T. H.

IM7/LARC(tm) MPEI-1 Polymide Composites

LARC(Trademark) MPEI-1 (Langley Research Center(Trademark) modified phenylethynyl imide-1) phenylethynyl containing aromatic polymide, is based on the reaction of biphenyl dianhydride (BPDA), 3,4'-oxydianiline (3,4'-ODA), 1,3-bis(3-aminophenoxy)benzene (APB), 2,4,6-triaminopyrimidine (TAP) and 4-phenylethynyl phthalic anhydride (PEPA), presumably resulting in a mixture of linear, branched and star shaped phenylethynyl containing imides which was evaluated as a matrix for high-performance composites. The poly(amid acid) solution of MPEI-1 in N-methypyrrolidinone was synthesized at 35% and 42% solids. Unidirectional prepreg was fabricated from these solutions and Hercules IM7 carbon fiber utilizing NASA- Langley's multipurpose prepreg machine. The temperature-dependent volatile depletion rates, thermal crystallization behavior and resin theology were characterized. Based on this information, a composite molding cycle was developed which yielded well consolidated, void-free laminates. Composite mechanical properties such as short beam shear strength, longitudinal and transverse flexural strength and flexural modulus, longitudinal tensile strength and notched and unnotched compression strengths were measured at room temperature (RT) and elevated temperatures. These mechanical properties are compared with those of IM7/LARC(Trademark) PETI-5 composites.

Hou, T. H.

Synthesis and Characterization of Modified Phenylethynyl Imides

As an ongoing effort to develop structural adhesives for high-performance aerospace applications, recent work has focused on phenylethynyl terminated imide (PETI) oligomers. The work reported herein involves the synthesis and characterization of a series of phenylethynyl containing oligomers designated LARC(TM) MPEI (modified phenylethynyl imide). These oligomers presumably contain mixtures of linear, branched and star-shaped molecules. The fully imidized polymers exhibited minimum melt viscosities as low as 600 poise at 335 C, significantly lower than equivalent molecular weight linear materials. Ti/Ti lap shear specimens processed at 288 C under 15 psi showed tensile shear strengths as high as approx. 6000 psi and 5200 psi at ambient temperature and 177 C respectively. The chemistry and properties of these new MPEIs are presented and compared with an optimized linear PETI, LARC(TM)PETI-5.

Jensen, B. J.

Free Volume in Glassy Poly(arylene Ether Ketone)s

Amorphous polyarylene ether ketones were examined in the glassy state by positron annihilation lifetime spectroscopy ( PALS ) and in the melt by standard rheological techniques. Specimens were well-characterized fractions of two isomeric structures. PALS clearly shows that the polymer with meta linkages in its backbone contains larger voids (greater than 0.25 nm radius). Thus despite their similar bulk densities, the two materials must pack very differently on a local scale. On the other hand, the free volumes inferred from the WLF treatment of melt viscosity data are practically identical in both materials ca. 4% at T(sub g). The comparison between techniques sheds some light on the distribution of free volume.

Hinkley, J. A.

Synthesis of imide/arylene ether copolymers for adhesives and composite matrices

A series of imide/arylene ether copolymers were prepared from the reaction of an amorphous arylene ether oligomer and a semi-crystalline imide oligomer. These copolymers were thermally characterized and mechanical properties were measured. One block copolymer was endcapped and the molecular weight was controlled to provide a material that displayed good compression moldability and attractive adhesion and composite properties.

Jensen, B. J.

Imide/arylene ether block copolymers

Two series of imide/arylene either block copolymers were prepared using an arylene ether block and either an amorphous or semi-crystalline imide block. The resulting copolymers were characterized and selected physical and mechanical properties were determined. These results, as well as comparisons to the homopolymer properties, are discussed.

Jensen, B. J.

Imide/arylene ether copolymers. I

The preparation of a series of novel imide/arylene ether copolymers is described together with the results of viscosity and DSC Tg(Tm) measurements. The copolymers were synthesized from an arylene ether block and either an amorphous or semicrystalline imide block. One block copolymer was end-capped, and the molecular weight was controlled to improve compression moldability. The paper also presents results of mechanical properties tests on copolymer samples.

Jensen, B. J.

Tough poly(arylene ether) thermoplastics as modifiers for bismaleimides

Several aspects of research on thermoplastics as toughness modifiers are discussed, including the contribution of the backbone chemistry and the concentration of the poly(arylene ether) thermoplastic to fracture toughness, influence of the molecular weight of the poly(arylene ether) thermoplastic on neat resin fracture toughness, and the morphology of the thermoplastic modified networks. The results show that fracture toughness of brittle bismaleimide resins can be improved significantly with poly(arylene ether) thermoplastic levels of 20 percent by weight, and that high molecular weight poly(arylene ether) based on bisphenol A provides the highest degree of toughening. Preliminary composite evaluation shows that improvements in neat resin toughness translate into carbon fabric composite.

Stenzenberger, H. D.

The 5-(4-Ethynylophenoxy) isophthalic chloride

Sulfone-ester polymers containing pendent ethynyl groups and a direct and multistep process for preparing them are disclosed. The multistep process involves the conversion of a pendent bromo group to the ethynyl group while the direct route involves reating hydroxy-terminated sulfone oligomer or polymers with a stoichiometric amount of 5-(4-ethynylphenoxy) isophthaloyl chloride. The 5-(4-ethynylphenoxy) isophthaloyl chloride and the process for preparing it are also disclosed.

Hergenrother, P. M.

Sulfone/Ester Polymers Containing Pendent Ethynyl Groups

Two processes make high-performance polymers resistant to solvents, without compromising mechanical characteristics. Polymers show improved solvent resistance while retaining high toughness, thermoformability, and mechanical performance. Multistep process involves conversion of pendent bromo group to ethynyl group, while direct process involves reacting hydroxy-terminated sulfone oligomers or polymers with stoichiometric amount of 5-(4-ethynylphenoxy) isophthaloyl chloride. Applications for new polymers include adhesives, composite resin matrices, moldings, ultrafiltration membranes, protective coatings, and such electrical insulators as thin films for microelectronic circuitry.

Hergenrother, P. M.

Polyarylene Ethers with Improved Properties

This invention relates to novel polyarylene ethers which possess the combination of high strength, toughness, and high use temperature with ease of extrusion and formation into complex objects. These polyarylene ethers are suitable for use in adhesives, coatings, films, membranes, and composite matrices. The polyarylene ethers of this invention are the polycondensation products from the reaction of either 1,3-bis (4-chloro or fluorobenzoyl) benzene with any one of the following bisphenolic compounds: bis (3-hydroxyphenyl) methane; bis (4-hydroxyphenyl) methane; 1,1-dimethyl-bis (4-hydroxyphenyl)methane, or 9,9-bis (4-hydroxyphenyl) fluorene. Random and block copolymers are also comprehended.

Hergenrother, P. M.

Melt-Pressed Films of Insoluble Semicrystalline Polymers

Technique known as "melt pressing" produces films from solid, insoluble, semicrystalline polymers in less than 5 minutes. Amount of crystallinity and possibly final crystal structure of film controlled in process. Induction heating, using gapped toroidal core, melts sample. Toroidal core and capacitor form tuned circuit. Below induction heating toroid, layer of insulation prevents heat transfer from insoluble film to induction heating apparatus.

Tyeryar, J. R.

New polyarylene ethers

A series of new polyarylene ethers (PAEs) were prepared from the reaction of activated dihalo compounds with various bisphenols. Measured number average molecular weights for the PAEs ranged from 13,500 to 39,400 g/mole, and glass transition temperatures varied from 152 to 280 C. Ethynyl-terminated polyarylene ethers (ETPAEs) were also prepared by endcapping hydroxy-terminated polyarylene ethers with 4-ethynylbenzoyl chloride. Structure/property relationships for the PAEs, and the advantages offered by the ETPAEs, are discussed.

Hergenrother, P. M.

Solvent Resistant Thermoplastic Composite Matrices

The following approaches improved the solvent resistance and raised the Tg of thermoplastics: end-capping aligomers with ethynyl groups; incorporating ethynyl groups pendent along the polymer chain; and correcting polymers containing pendent ethynyl groups with a low molecular weight diethynyl compound. The following conclusions were reached: (1) film and composite properties off an ethynyl-terminated sulfone were better than those of UDEL (trademark); (2) fracture energy of an ethynyl-terminated sulfone was lower than that of UDEL (trademark); (3) residual palladium in the cured ethynyl-terminated sulfone lower the thermooxidative stability of the cured resin; (4) the properties of a phenoxy resin were altered considerably by placing pendent ethynyl groups along the polymer chain; and (5) property trade-offs must be considered when thermoplastics are modified via reactant groups.

Hergenrother, P. M.

Thermoplastic composite matrices with improved solvent resistance

In order to improve solvent resistance of aromatic thermoplastic polymers, ethynyl-terminated aromatic sulfone polymers (ETS), sulfone/ester polymers (SEPE) containing pendent ethynyl groups, and phenoxy resin containing pendent ethynyl groups are synthesized. Cured polysulfones and phenoxy resins containing ethynyl groups on the ends or pendent on the molecules exhibited systematic behavior in solvent resistance, film flexibility, and toughness as a function of crosslink density. The film and composite properties of a cured solvent-resistant ETS were better than those of a commercially available solvent sensitive polysulfone. The study was part of a NASA program to better understand the trade-offs between solvent resistance, processability and mechanical properties which may be useful in designing composite structures for aerospace vehicles.

Hergenrother, P. M.

Phenoxy resins containing pendent ethynyl groups

As part of an effort on tougher/solvent resistant matrix resins for composites, research was directed towards exploring methods to improve the solvent resistance of linear amorphous thermoplastics. Ethyl reactive groups were placed on the ends of oligomers and pendent along the polymer chain and subsequently thermally reacted to provide crosslinking and thus improvement in solvent resistance. This concept is extended to another thermoplastic, a phenoxy resin. A commercially available phenoxy resin (PKHH) was systematically modified by reaction of the pendent hydroxyl groups on the phenoxy resin with various amounts of 4-ethynylbenzoyl chloride. As the pendent ethynyl group content in the phenoxy resin increased, the cured resin exhibited a higher glass transition temperature, better solvent resistance and less flexibility. The solvent resistance was further improved by correcting a low molecular weight diethynyl compound, 2,2-bis(4-ethynylbenzoyloxy-4'-phenyl)propane, with a phenoxy resin containing pendent ethynyl groups.

Hergenrother, P. M.

Polyimide characterization studies - Effect of pendant alkyl groups

The effect on selected polyimide properties when pendant alkyl groups were attached to the polymer backbone was investigated. A series of polymers were prepared using benzophenone tetracarboxylic acid dianhydride (BTDA) and seven different p-alkyl-m,p'-diaminobenzophenone monomers. The alkyl groups varied in length from C(1) (methyl) to C(9) (nonyl). The polyimide prepared from BTDA and m,p'-diaminobenzophenone was included as a control. All polymers were characterized by various chromatographic, spectroscopic, thermal, and mechanical techniques. Increasing the length of the pendant alkyl group resulted in a systematic decrease in glass transition temperature (Tg) for vacuum cured films. A 70 C decrease in Tg to 193 C was observed for the nonyl polymer compared to the Tg for the control. A corresponding systematic increase in Tg indicative of crosslinking, was observed for air cured films. Thermogravimetric analysis revealed a slight sacrifice in thermal stability with increasing alkyl length. No improvement in film toughness was observed.

Jensen, B. J.

Polyimides with pendant alkyl groups

The effect on selected polyimide properties when pendant alkyl groups were attached to the polymer backbone was investigated. A series of polymers were prepared using benzophenone tetracarboxylic acid dianhydride (BTDA) and seven different p-alkyl-m,p'-diaminobenzophenone monomers. The alkyl groups varied in length from C(1) (methyl) to C(9) (nonyl). The polyimide prepared from BTDA and m,p'-diaminobenzophenone was included as a control. All polymers were characterized by various chromatographic, spectroscopic, thermal, and mechanical techniques. Increasing the length of the pendant alkyl group resulted in a systematic decrease in glass transition temperature (Tg) for vacuum cured films. A 70 C decrease in Tg to 193 C was observed for the nonyl polymer compared to the Tg for the control. A corresponding systematic increase in Tg indicative of crosslinking, was observed for air cured films. Thermogravimetric analysis revealed a slight sacrifice in thermal stability with increasing alkyl length. No improvement in film toughness was observed.

Jensen, B. J.