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At least 829 records · Page 46

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NASA NTRS2004

Diels-Alder Trapping of Photochemically Generated o-Quinodimethane Intermediates: An Alternative Route to Photocured Polymer Film Development

Photolysis of o-methylphenyl ketones generates bis-o-quinodimethane intermediates that can be trapped in situ by dienophiles through Diels-Alder cycloadditions. This well-known photochemical process is applied to a series of six new photoreactive monomers containing bis-(o-methylphenyl ketone) functionalities combined with diacrylate and triacrylate ester monomers for the development of acrylic ester copolymer blends. Irradiation of cyclohexanone solutions of the bis-(o-methylphenyl ketone)s and acrylate esters produce thin polymer films. Solid state 13C NMR data indicated 47- 100% reaction of the bis-(o-methylphenyl ketone)s, depending on experimental conditions, to yield the desired products. DSC and TGA analyses were performed to determine the glass transition temperature, T,, and onset of decomposition, Td, of the resulting polymer films. A statistical Design of Experiments approach was used to obtain a systematic understanding of the effects of experimental variables on the extent of polymerization and the final polymer properties.

Tyson, Daniel S.↗

NASA NTRS2005

Liquid Crystalline Thermosets from Ester, Ester-Imide, and Ester-Amide Oligomers

Main chain thermotropic liquid crystal esters, ester-imides, and ester-amides were prepared from AA, BB, and AB type monomeric materials and were end-capped with phenylacetylene, phenylmaleimide, or nadimide reactive end-groups. The resulting reactive end-capped liquid crystal oligomers exhibit a variety of improved and preferred physical properties. The end-capped liquid crystal oligomers are thermotropic and have, preferably, molecular weights in the range of approximately 1000-15,OOO grams per mole. The end-capped liquid crystal oligomers have broad liquid crystalline melting ranges and exhibit high melt stability and very low melt viscosities at accessible temperatures. The end-capped liquid crystal oligomers are stable for up to an hour in the melt phase. These properties make the end-capped liquid crystal oligomers highly processable by a variety of melt process shape forming and blending techniques including film extrusion, fiber spinning, reactive injection molding (RIM), resin transfer molding (RTM), resin film injection (RFI), powder molding, pultrusion, injection molding, blow molding, plasma spraying and thermo-forming. Once processed and shaped, the end- capped liquid crystal oligomers were heated to further polymerize and form liquid crystalline thermosets (LCT). The fully cured products are rubbers above their glass transition temperatures. The resulting thermosets display many properties that are superior to their non-end-capped high molecular weight analogs.

Theodornus J Dingemans↗

NASA NTRS2006

Chemical, Physical, and Mechanical Characterization of Isocyanate Cross-linked Amine-Modified Silica Aerogels

We describe a new mechanically strong lightweight porous composite material obtained by encapsulating the skeletal framework of amine-modified silica aerogels with polyurea. The conformal polymer coating preserves the mesoporous structure of the underlying silica framework and the thermal conductivity remains low at 0.041 plus or minus 0.001 W m(sup -1 K(sup -1). The potential of the new cross-linked silica aerogels for load-carrying applications was determined through characterization of their mechanical behavior under compression, three-point bending, and dynamic mechanical analysis (DMA). A primary glass transition temperature of 130 C was identified through DMA. At room temperature, results indicate a hyperfoam behavior where in compression cross-linked aerogels are linearly elastic under small strains (less than 4%) and then exhibit yield behavior (until 40% strain), followed by densification and inelastic hardening. At room temperature the compressive Young's modulus and the Poisson's ratio were determined to be 129 plus or minus 8 MPa and 0.18, respectively, while the strain at ultimate failure is 77% and the average specific compressive stress at ultimate failure is 3.89 x 10(exp 5) N m kg(sup -1). The specific flexural strength is 2.16 x 10(exp 4) N m kg(sup -1). Effects on the compressive behavior of strain rate and low temperature were also evaluated.

Katti, Atul↗

NASA NTRS2006

Ground Testing A 20-Meter Inflation Deployed Solar Sail

Solar sails have been proposed for a variety of future space exploration missions and provide a cost effective source of propellantless propulsion. Solar sails span very large areas to capture and reflect photons from the Sun and are propelled through space by the transfer of momentum from the photons to the solar sail. The thrust of a solar sail, though small, is continuous and acts for the life of the mission without the need for propellant. Recent advances in materials and ultra-low mass gossamer structures have enabled a host of useful space exploration missions utilizing solar sail propulsion. The team of L Garde, NASA Jet Propulsion Laboratory (JPL), Ball Aerospace, and NASA Langley Research Center, under the direction of the NASA In-Space Propulsion Office (ISP), has been developing a scalable solar sail configuration to address NASA s future space propulsion needs. The 100-m baseline solar sail concept was optimized around the one astronomical unit (AU) Geostorm mission, and features a Mylar sail membrane with a striped-net sail suspension architecture with inflation-deployed sail support beams consisting of inflatable sub-Tg (glass transition temperature) rigidizable semi-monocoque booms and a spreader system. The solar sail has vanes integrated onto the tips of the support beams to provide full 3-axis control of the solar sail. This same structural concept can be scaled to meet the requirements of a number of other NASA missions. Static and dynamic testing of a 20m scaled version of this solar sail concept have been completed in the Space Power Facility (SPF) at the NASA Glenn Plum Brook facility under vacuum and thermal conditions simulating the operation of a solar sail in space. This paper details the lessons learned from these and other similar ground based tests of gossamer structures during the three year solar sail project.

Mann, Troy↗

NASA NTRS1995

(abstract) Determination of the Specific Heat and Total Hemispherical Total Emissivity of the Highly Undercooled Zr(sub 41.2)Ti(sub 13.8)Cu(sub 12.5)Ni(sub 10.0)Be(sub 22.5) Alloy

High temperature high vacuum electrostatic levitation was combined with DSC experiments to determine the specific heat C(sub p) of the undercooled Zr(sub 41.2)Ti(sub 13.8)Cu(sub 12.5)Ni(sub 10.0)Be(sub 22.5) liquid as a function of temperature. The containerless approach made it possible to undercool the melt to the glass transition temperature without inducing nucleation. Because the cooling process was purely radiative, noncontact temperature measurement techniques could be used to determine the specific heat to total hemispherical emissivity ratio, C(sub p)/epsilon(sub t), for the undercooled liquid region. Using C(sub p) values which were independently obtained by DSC, epsilon(sub t) could be determined. With knowledge of C(sub p) of the undercooled liquid it was possible to determine other thermodynamic properties such as Gibbs free energy and entropy as a function of undercooling.

levitation thermodynamic properties undercooled al↗

NASA NTRS2006

Nitrile/Buna N Material Failure Assessment for an O-Ring used on the Gaseous Hydrogen Flow Control Valve (FCV) of the Space Shuttle Main Engine

After the rollout of Space Shuttle Discovery in April 2005 in preparation for return-to-flight, there was a failure of the Orbiter (OV-103) helium signature leak test in the gaseous hydrogen (GH2) system. Leakage was attributed to the Flow Control Valve (FCV) in Main Engine 3. The FCV determined to be the source of the leak for OV-103 is designated as LV-58. The nitrile/Buna N rubber O-ring seal was removed from LV-58, and failure analysis indicated radial cracks providing leak paths in one quadrant. Cracks were eventually found in 6 of 9 FCV O-rings among the three Shuttle Orbiters, though none were as severe as those for LV-58, OV-103. Testing by EM10 at MSFC on all 9 FCV O- rings included: laser dimensional, Shore A hardness and properties from a dynamic mechanical analyzer (DMA) and an Instron tensile machine. The following test data was obtained on the cracked quadrant of the LV-58, OV-103 O-ring: (1) the estimated compression set was only 9.5%, compared to none for the rest of the O-ring; (2) Shore A hardness for the O.D. was higher by almost 4 durometer points than for the rest of the O-ring; and (3) DMA data showed that the storage/elastic modulus E was almost 25% lower than for the rest of the O-ring. Of the 8 FCV O-rings tested on an Instron, 4 yielded tensile strengths that were below the MIL spec requirement of 1350 psi-a likely influence of rubber cracking. Comparisons were made between values of modulus determined by DNA (elastic) and Instron (Young s). Each nitrile/Buna N O-ring used in the FCV conforms to the MIL-P-25732C specification. A number of such O-rings taken from shelf storage at MSFC and Kennedy Space Center (KSC) were used to generate a reference curve of DMA glass transition temperature (Tg) vs. shelf storage time ranging from 8 to 26 years. A similar reference curve of TGA onset temperature (of rubber weight loss) vs. shelf storage time was also generated. The DMA and TGA data for the used FCV O-rings were compared to the reference curves. Correlations were also made between the DMA modulus (at 22 C) and Shore A hardness for all 9 of the FCV O-rings used among the three Shuttle Orbiters. The radial cracking in the FCV O-rings was determined to be due to ozone attack, as nitrile/Buna N rubber is susceptible to such attack. Nitrile/Buna N material under MIL-P25732C should be used in a hydraulic fluid environment to help protect it from cracking. However, the FCV O-rings were used in an air only environment. The FCV design has as much as a 9-mil gap that allows the O.D. of the O-ring to be directly exposed to ozone, pressurized air and some elevated temperatures, accelerating the weathering process that leads to O-ring cracking. Space Shuttle flights will likely not continue past 2010. Therefore, Shuttle management decided to continue using the nitrile/Buna N material for the FCVs, but have each O-ring replaced after 3 years to minimize any chances for crack initiation.

Wingard, Doug↗

NASA NTRS2006

Space Environmentally Durable Polyimides and Copolyimides

Polyimides displaying low color in thin films, atomic oxygen resistance, vacuum ultraviolet radiation resistance, solubility in organic solvents in the imide form, high glass transition (T(sub g)) temperatures, and high thermal stability are provided. The poly(amide acid)s, copoly(amide acid)s, polyimides and copolyimides are prepared by the reaction of stoichiometric ratios of an aromatic &anhydride with diamines which contain phenylphosphine oxide groups in polar aprotic solvents. Controlled molecular weight oligomeric (amide acid)s and imides can be prepared by offsetting the stoichiometry according to the Carothers equation using excess diamine and endcapping with aromatic anhydrides. The polyimide materials can be processed into various material forms such as thin films, fibers, foams, threads, adhesive film, coatings, dry powders, and fiber coated prepreg, and uses include thin film membranes on antennas, second-surface mirrors, thermal optical coatings, and multilayer thermal insulation (MLI) blanket materials.

Connell, John W.↗

NASA NTRS2007

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.↗

NASA NTRS2006

Advanced Polymers Containing the Phenyltrifluoroethylidene Connecting Group

A new, lower cost fluorinated dianhydride based on the phenyltrifluoroethylidene (3F) connecting linkage was invented by the principal author in the early 1980's. New 3F condensation and addition cured polyimides were synthesized with the newly discovered 3F dianhydride and the previously known 3F diamine. As controls, polyimides based on the somewhat analogous higher cost hexafluoroisopropylidene (6F) linkage were also prepared. The short term thermal oxidative stability (TOS), determined by thermal gravimetric analysis (TGA), and the glass transition temperatures (Tg) of 3F dianhydride polyimides were found to be similar to 6F dianhydride polyimides, but the Tg was slightly higher for 3F diamine polyimides than 6F diamine polyimides. Unfortunately, in real time testing, long term TOS of 3F polymers was clearly inferior to 6F polymers. This was due to a 3 to 5 fold greater rate of loss of trifluoromethyl group from 3F versus 6F linkages. However, at shorter times or lower temperatures, 3F TOS was almost comparable to 6F TOS. The wide scope of the 3F technology was also demonstrated to have distinct unique advantages over 6F technology through the use of the 3F pendant phenyl ring as a synthetic site to introduce other functional groups. These groups have been used for the control or modification of polymer properties; an advantage lacking within 6F technology. The synthetic ease by which 3F can be introduced into various types of monomers has lead to the explosion of advanced 3F polyimides and other high performance advanced 3F polymers in the prior decade of 3F polymer literature as cited herein; covering polyimides, substituted polyimides, at least ten types of nonpolyimide 3F polymer modifications, and also the government's nine 3F U.S. patents and corporations' nine 3F U.S. patents.

Alstron, William B.↗

NASA NTRS1994

Polybenzimidazole via aromatic nucleophilic displacement

Di(hydroxyphenyl)benzimidazole monomers were prepared from phenyl-4-hydroxybenzoate and aromatic bis(o-diamine)s. These monomers were used in the synthesis of soluble polybenzimidazoles. The reaction involved the aromatic nucleophilic displacement of various di(hydroxyphenyl)benzimidazole monomers with activated aromatic dihalides or activated aromatic dinitro compounds in the presence of an alkali metal base. These polymers exhibited lower glass transition temperatures, improved solubility, and better compression moldability over their commercial counterparts.

Connell, John W.↗

NASA NTRS2002

Copolymer sealant compositions and method for making

Condensation curable poly(fluoroorgano)siloxane-poly(silarylene)siloxane block copolymer compositions having a glass transition temperature not exceeding about -54.degree. C. and excellent solvent resistance have been found useful as sealants. Polyalkoxysilylorgano compounds, such as 1,4-bis[trimethoxysilyl(ethyl)]benzene have been found to be effective as cross-linkers.

Singh, Navjot↗

NASA NTRS2005

Liquid crystalline thermosets from ester, ester-imide, and ester-amide oligomers

Main chain thermotropic liquid crystal esters, ester-imides, and ester-amides were prepared from AA, BB, and AB type monomeric materials and were end-capped with phenylacetylene, phenylmaleimide, or nadimide reactive end-groups. The resulting reactive end-capped liquid crystal oligomers exhibit a variety of improved and preferred physical properties. The end-capped liquid crystal oligomers are thermotropic and have, preferably, molecular weights in the range of approximately 1000-15,000 grams per mole. The end-capped liquid crystal oligomers have broad liquid crystalline melting ranges and exhibit high melt stability and very low melt viscosities at accessible temperatures. The end-capped liquid crystal oligomers are stable for up to an hour in the melt phase. These properties make the end-capped liquid crystal oligomers highly processable by a variety of melt process shape forming and blending techniques including film extrusion, fiber spinning, reactive injection molding (RIM), resin transfer molding (RTM), resin film injection (RFI), powder molding, pultrusion, injection molding, blow molding, plasma spraying and thermo-forming. Once processed and shaped, the end-capped liquid crystal oligomers were heated to further polymerize and form liquid crystalline thermosets (LCT). The fully cured products are rubbers above their glass transition temperatures. The resulting thermosets display many properties that are superior to their non-end-capped high molecular weight analogs.

Dingemans, Theodorous J.↗

NASA NTRS2004

Copolymer sealant compositions and method for making

Singh, Navjot↗

NASA NTRS1998

Processes for treating cellulosic material

Disclosed are processes for pretreating cellulosic materials in liquid water by heating the materials in liquid water at a temperature at or above their glass transition temperature but not substantially exceeding 220.degree. C., while maintaining the pH of the reaction medium in a range that avoids substantial autohydrolysis of the cellulosic materials. Such pretreatments minimize chemical changes to the cellulose while leading to physical changes which substantially increase susceptibility to hydrolysis in the presence of cellulase.

Ladisch, Michael R.↗

NASA NTRS2003

Copolymer sealant compositions and method for making

Singh, Navjot↗

NASA NTRS1995

Solvent resistant copolyimide

A solvent resistant copolyimide was prepared by reacting 4,4'-oxydiphthalic anhydride with a diaimine blend comprising, based on the total amount of the diamine blend, about 75 to 90 mole percent of 3,4'-oxydianiline and about 10 to 25 mole percent p-phenylene diamine. The solvent resistant copolyimide had a higher glass transition temperature when cured at 350.degree. , 371.degree. and 400.degree. C. than LaRC.TM.-IA. The composite prepared from the copolyimide had similar mechanical properties to LaRC.TM.-IA. Films prepared from the copolyimide were resistant to immediate breakage when exposed to solvents such as dimethylacetamide and chloroform. The adhesive properties of the copolyimide were maintained even after testing at 23.degree., 150.degree., 177.degree. and 204.degree. C.

Chang, Alice C.↗

NASA NTRS2008

Low Viscosity Imides Based on Asymmetric Oxydiphthalic Anhydride

A series of low-melt viscosity imide resins were prepared from asymmetric oxydiphthalic dianhydride (a-ODPA) and 4-phenylethynylphthalic anhydride as the endcap, along with 3,4' - oxydianiline (3,4' -ODA), 3,4' -methylenedianiline (3,4' -MDA), 3,3' -methylenedianiline (3,3' - MDA) and 3,3'-diaminobenzophenone (3,3'-DABP), using a solvent-free melt process. These imide oligomers displays low-melt viscosities (2-15 poise) at 260-280 C, which made them amenable to low-cost resin transfer molding (RTM) process. The a-ODPA based RTM resins exhibits glass transition temperatures (Tg's) in the range of 265-330 C after postcure at 343 C. The mechanical properties of these polyimide/carbon fiber composites fabricated by RTM will be discussed.

Chuang, Kathy C.↗

NASA NTRS2008

Kevlar 49/Epoxy COPV Aging Evaluation

NASA initiated an effort to determine if the aging of Kevlar 49/Epoxy composite overwrapped pressure vessels (COPV) affected their performance. This study briefly reviews the history and certification of composite pressure vessels employed on NASA Orbiters. Tests to evaluate overwrap tensile strength changes compared 30 year old samples from Orbiter vessels to new Kevlar/Epoxy pressure vessel materials. Other tests include transverse compression and thermal analyses (glass transition and moduli). Results from these tests do not indicate a noticeable effect due to aging of the overwrap materials.

Sutter, James K.↗