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All sourcesNASA NTRSDOE OSTI
NASA NTRS2003

Quantification Of Fire Signatures For Practical Spacecraft Materials

The overall objective of this project is to measure the fire signatures of typical spacecraft materials in 1-g and determine how these signatures may be altered in a microgravity environment. During this project, we will also develop a test technique to obtain representative low-gravity signatures. The specific tasks that will be accomplished to achieve these objectives are to: (1) measure the time history of various fire signatures of typical spacecraft materials in 1-g at varying heating rates, temperatures, convective velocities, and oxygen concentrations, (2) conduct tests in the Zero-Gravity Facility at NASA John H. Glenn Research Center to investigate the manner that a microgravity environment alters the fire signature,(3) compare 0-g and 1-g time histories and determine if 0-g data exhibits the same dependence on the test parameters as experienced in 1-g (4) develop a 1-g test technique by which 0-g fire signatures can be measured. The proposed study seeks to investigate the differences in the identities and relative concentrations of the volatiles produced by pyrolyzing and/or smoldering materials between normal gravity and microgravity environments. Test materials will be representative of typical spacecraft materials and, where possible, will be tested in appropriate geometries. Wire insulation materials of Teflon, polyimide, silicone, and PVC will be evaluated using either cylindrical samples or actual wire insulation. Other materials such as polyurethane, polyimide, melamine, and silicone-based foams will be tested using cylindrical samples, in addition to fabric materials, such as Nomex. Electrical components, such as resistors, capacitors, circuit board will also be tested.

VanderWal, Randy L.↗
NASA NTRS2004

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.↗
NASA NTRS2004

Polyimide/Carbon Nanotube Composite Films for Electrostatic Charge Mitigation

Low color, space environmentally durable polymeric films with sufficient electrical conductivity to mitigate electrostatic charge build-up have been under investigation as part of a materials development activity. In the work described herein, single-walled carbon nanotubes (SWNT) solutions were dispersed in solutions of a novel ionomer in N,N-dimethylacetamide resulting in homogenous suspensions or quasi-solutions. The ionomer was used to aid in the dispersal of SWNTs in to a soluble, low color space environmentally durable polyimide. The use of the ionomer as a dispersant enabled the nanotubes to be dispersed at loading levels up to 3 weight % in a polyimide solution without visual agglomeration. The films were further characterized for their electrical and mechanical properties.

Delozier, D. M.↗
NASA NTRS2004

Laboratory Analysis of Polymer Thin Films for Planetary Balloons and Gossamer Structures

Commercially available polymer thin fdms with thickness of 15 microns or less were evaluated for potential application as the gas envelope material of balloons and other inflated vehicles. Films on this thickness scale are of interest for Earth and Mars ballooning as well as many gossamer space structures. Due to the uniqueness of these missions relative to typical uses of these materials, application-specific materials properties measurements were made. We evaluated numerous polymer chemistries, plus a few variations within one chemistry. The data show that there are often trade-offs among the different materials, such as with polyesters and polyimides having greater stiffness (modulus) but lower tear propagation resistance than polyethylene. Sections of polyethylene films can be joined by heat sealing, while adhesives and their accompanying mass penalty must be used with polyesters and polyimides. When the analysis temperature is reduced to 190 K, polyethylenes display dramatically increased stiffness and yield point, while the increase for other materials is more modest. The data also show that manufacturing processes can significantly affect film properties. To emphasize the need for application-specific properties assessment, we discuss two recent applications using these materials.

Sterling, Jerry↗
NASA NTRS2002

Fabrication and Electromagnetic Characterization of Novel Self-Metallized Thin Films

Unique, self-metallized films were investigated for deployable reflector antenna applications at L-band. Polyamic acid resins or soluble polyimides were doped with metal complexes, cast into films, and thermally cured. Each resulting film had a metallic layer on one side, adhering unfailingly to the polymer. Metallization was successful for silver or palladium in 3,3',4,4'-benzophenonetetracarboxylic acid dianhydride (BTDA) and 4,4'- oxydianiline and for gold in BTDA and 2,2-bis[4-(4- aminophenoxy)phenyl]hexafluoropropane (4-BDAF) or the space durable polyimide, 2,2-bis(3,4-dicarboxyphenyl)- hexafluoropropane dianhydride and 4-BDAF (LaRCCP1). Reflectivity, transmissivity, and emissivity were determined, using an HP 8510 Vector Network Analyzer, to within 0.001 precision and accuracy. A custom-made test fixture/positioner, a thru-reflect-line calibration, and calculated reflection coefficients were used. The Ag film proved most suitable for further study, with 0.9957 reflectivity and 0.0042 emissivity. The Pd films were 0.89 reflective and 0.11 emissive; both Au films tested entirely transmissive. Transmission and scanning electron micrographs, S-parameters, and power coefficients are shown.

Mackenzie, Anne I.↗
NASA NTRS2001

Investigating the Use of Ultrasound for Evaluating Aging Wiring Insulation

This paper reviews our initial efforts to investigate the use of ultrasound to evaluate wire insulation. Our initial model was a solid conductor with heat shrink tubing applied. In this model, various wave modes were identified. Subsequently, several aviation classes of wires (MIL-W- 81381, MIL-W-22759/34, and MIL-W-22759/87) were measured. The wires represented polyimide and ethylene-tetraflouroethylene insulations, and combinations of polyimide and flouropolymer plastics. Wire gages of 12, 16, and 20 AWG sizes were measured. Finally, samples of these wires were subjected to high temperatures for short periods of time to cause the insulation to degrade. Subsequent measurements indicated easily detectable changes.

Madaras, Eric I.↗
NASA NTRS2003

The Evaluation of High Temperature Adhesive Bonding Processes for Rocket Engine Combustion Chamber Applications

NASA Glenn Research Center is currently evaluating the possibility of using high- temperature polymer matrix composites to reinforce the combustion chamber of a rocket engine. One potential design utilizes a honeycomb structure composed of a PMR-II- 50/M40J 4HS composite facesheet and titanium honeycomb core to reinforce a stainless steel shell. In order to properly fabricate this structure, adhesive bond PMR-II-50 composite. Proper prebond surface preparation is critical in order to obtain an acceptable adhesive bond. Improperly treated surfaces will exhibit decreased bond strength and durability, especially in metallic bonds where interface are susceptible to degradation due to heat and moisture. Most treatments for titanium and stainless steel alloys require the use of strong chemicals to etch and clean the surface. This processes are difficult to perform due to limited processing facilities as well as safety and environmental risks and they do not consistently yield optimum bond durability. Boeing Phantom Works previously developed sol-gel surface preparations for titanium alloys using a PETI-5 based polyimide adhesive. In support of part of NASA Glenn Research Center, UDRI and Boeing Phantom Works evaluated variations of this high temperature sol-gel surface preparation, primer type, and primer cure conditions on the adhesion performance of titanium and stainless steel using Cytec FM 680-1 polyimide adhesive. It was also found that a modified cure cycle of the FM 680-1 adhesive, i.e., 4 hrs at 370 F in vacuum + post cure, significantly increased the adhesion strength compared to the manufacturer's suggested cure cycle. In addition, the surface preparation of the PMR-II-50 composite was evaluated in terms of surface cleanness and roughness. This presentation will discuss the results of strength and durability testing conducted on titanium, stainless steel, and PMR-II-50 composite adherends to evaluate possible bonding processes.

McCray, Daniel↗
NASA NTRS2003

Effect of Sizings on the Durability of High Temperature Polymer Composites

To increase performance and durability of high-temperature composite for potential rocket engine components, it is necessary to optimize wetting and interfacial bonding between high modulus carbon fibers and high-temperature polyimide resins. Sizing commercially supplied on most carbon fiber are not compatible with polyimides. In this study, the chemistry of sizing on two high modulus carbon fiber (M40J and M60J, Tiray) was characterized. A continuous desizling system that uses an environmentally friendly chemical-mechanical process was developed for tow level fiber. Composites were fabricated with fibers containing the manufacturer's sizing, desized, and further treated with a reactive finish. Results of room-temperature tests after thermal aging show that the reactive finish produces a higher strength and more durable interface compared to the manufacturer's sizing. When exposed to moisture blistering tests, however, the butter bonded composite displayed a tendency to delaminate, presumably due to trapping of volatiles.

Allred, Ronald E.↗
NASA NTRS1997

High-Temperature Adhesive Strain Gage Developed

Researchers at the NASA Lewis Research Center have developed a unique strain gage and adhesive system for measuring the mechanical properties of polymers and polymer composites at elevated temperatures. This system overcomes some of the problems encountered in using commercial strain gages and adhesives. For example, typical commercial strain gage adhesives require a postcure at temperatures substantially higher than the maximum test temperature. The exposure of the specimen to this temperature may affect subsequent results, and in some cases may be higher than the glass-transition temperature of the polymer. In addition, although typical commercial strain gages can be used for short times at temperatures up to 370 C, their long-term use is limited to 230 C. This precludes their use for testing some high-temperature polyimides near their maximum temperature capability. Lewis' strain gage and adhesive system consists of a nonencapsulated, unbacked gage grid that is bonded directly to the polymer after the specimen has been cured but prior to the normal postcure cycle. The gage is applied with an adhesive specially formulated to cure under the specimen postcure conditions. Special handling, mounting, and electrical connection procedures were developed, and a fixture was designed to calibrate each strain gage after it was applied to a specimen. A variety of tests was conducted to determine the performance characteristics of the gages at elevated temperatures on PMR-15 neat resin and titanium specimens. For these tests, which included static tension, thermal exposure, and creep tests, the gage and adhesive system performed within normal strain gage specifications at 315 C. An example of the performance characteristics of the gage can be seen in the figure, which compares the strain gage measurement on a polyimide specimen at 315 C with an extensometer measurement.

Pereira, J. Michael↗
NASA NTRS2005

High Performance Polymers and Composites (HiPPAC) Center

NASA University Research Centers funding has allowed Clark Atlanta University (CAU) to establish a High Performance Polymers and Composites (HiPPAC) Research Center. Clark Atlanta University, through the HiPPAC Center has consolidated and expanded its polymer and composite research capabilities through the development of research efforts in: (1) Synthesis and characterization of polymeric NLO, photorefractive, and piezoelectric materials; (2) Characterization and engineering applications of induced strain smart materials; (3) Processable polyimides and additives to enhance polyimide processing for composite applications; (4) Fabrication and mechanical characterization of polymer based composites.

Mintz, Eric A.↗
NASA NTRS2000

Chemical Fabrication Used to Produce Thin-Film Materials for High Power-to- Weight-Ratio Space Photovoltaic Arrays

The key to achieving high specific power (watts per kilogram) space solar arrays is the development of a high-efficiency, thin-film solar cell that can be fabricated directly on a flexible, lightweight, space-qualified durable substrate such as Kapton (DuPont) or other polyimide or suitable polymer film. Cell efficiencies approaching 20 percent at AM0 (air mass zero) are required. Current thin-film cell fabrication approaches are limited by either (1) the ultimate efficiency that can be achieved with the device material and structure or (2) the requirement for high-temperature deposition processes that are incompatible with all presently known flexible polyimide or other polymer substrate materials. Cell fabrication processes must be developed that will produce high-efficiency cells at temperatures below 400 degrees Celsius, and preferably below 300 degress Celsius to minimize the problems associated with the difference between the coefficients of thermal expansion of the substrate and thin-film solar cell and/or the decomposition of the substrate.

Hepp, Aloysius F.↗
NASA NTRS2002

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.↗
NASA NTRS2001

PMR Extended Shelf Life Technology Given 2000 R and D 100 Award

An approach developed at the NASA Glenn Research Center for extending the shelf life of PMR polyimide solutions and prepregs received an R&D 100 Award this year. PMR polyimides, in particular PMR-15, have become attractive materials for a variety of aerospace applications because of their outstanding high-temperature stability and performance. PMR-15 can be used in components with exposures to temperatures as high as 290 C, which leads to substantial reductions in weight, as much as 30 percent over metal components. PMR-15 composites are used widely in aerospace applications ranging from ducts and external components in aircraft engines to an engine access door for the Space Shuttle Main Engine. A major barrier to more widespread use of these materials is high component costs. Recent efforts at Glenn have addressed the various factors that contribute to these costs in an attempt to more fully utilize these lightweight, high-temperature materials.

Meador, Michael A.↗
NASA NTRS1990

Development of HVOF Sprayed Erosion/Oxidation Resistant Coatings for Composite Structural Components in Propulsion Systems

Thermally sprayed coatings are being studied and developed as methods of enabling lightweight composites to be used more extensively as structural components in propulsion applications in order to reduce costs and improve efficiency through weight reductions. The primary goal of this work is the development of functionally graded material [FGM] polymer/metal matrix composite coatings to provide improved erosion/oxidation resistance to polyimide-based polymer matrix composite [PMC] substrates. The goal is to grade the coating composition from pure polyimide, similar to the PMC substrate matrix on one side, to 100% WC-Co on the other. Both step-wise and continuous gradation of the loading of the WC-Co reinforcing phase are being investigated, Details of the coating parameter development will be presented, specifically the high velocity oxy-fuel [HVOF] combustion spraying of pure PMR-I1 matrix material and layers of various composition PMR-II/WC-Co blends onto steel and PMR-15 composite substrates. Results of the HVOF process optimization, microstructural characterization, and analysis will be presented. The sprayed coatings were evaluated using standard metallographic techniques - optical and scanning electron microscopy [SEMI. An SEM + electron dispersive spectroscopy [EDS] technique has also been used to confirm retention of the PMR-I1 component. Results of peel/butt adhesion testing to determine adhesion will also be presented.

Ivosevic, M.↗
NASA NTRS2006

Evaluation Of Risk And Possible Mitigation Schemes For Previously Unidentified Hazards

This report presents the results of arc track testing conducted to determine if such a transfer of power to un-energized wires is possible and/or likely during an arcing event, and to evaluate an array of protection schemes that may significantly reduce the possibility of such a transfer. The results of these experiments may be useful for determining the level of protection necessary to guard against spurious voltage and current being applied to safety critical circuits. It was not the purpose of these experiments to determine the probability of the initiation of an arc track event only if an initiation did occur could it cause the undesired event: an inadvertent thruster firing. The primary wire insulation used in the Orbiter is aromatic polyimide, or Kapton , a construction known to arc track under certain conditions [3]. Previous Boeing testing has shown that arc tracks can initiate in aromatic polyimide insulated 28 volts direct current (VDC) power circuits using more realistic techniques such as chafing with an aluminum blade (simulating the corner of an avionics box or lip of a wire tray), or vibration of an aluminum plate against a wire bundle [4]. Therefore, an arc initiation technique was chosen that provided a reliable and consistent technique of starting the arc and not a realistic simulation of a scenario on the vehicle. Once an arc is initiated, the current, power and propagation characteristics of the arc depend on the power source, wire gauge and insulation type, circuit protection and series resistance rather than type of initiation. The initiation method employed for these tests was applying an oil and graphite mixture to the ends of a powered twisted pair wire. The flight configuration of the heater circuits, the fuel/oxider (or ox) wire, and the RCS jet solenoid were modeled in the test configuration so that the behavior of these components during an arcing event could be studied. To determine if coil activation would occur with various protection wire schemes, 145 tests were conducted using various fuel/ox wire alternatives (shielded and unshielded) and/or different combinations of polytetrafuloroethylene (PTFE), Mystik tape and convoluted wraps to prevent unwanted coil activation. Test results were evaluated along with other pertinent data and information to develop a mitigation strategy for an inadvertent RCS firing. The SSP evaluated civilian aircraft wiring failures to search for aging trends in assessing the wire-short hazard. Appendix 2 applies Weibull statistical methods to the same data with a similar purpose.

Linzey, William↗
NASA NTRS2006

Mechanical Properties of T650-35/AFR-PE-4 at Elevated Temperatures for Lightweight Aeroshell Designs

Considerable efforts have been underway to develop multidisciplinary technologies for aeroshell structures that will significantly increase the allowable working temperature for the aeroshell components, and enable the system to operate at higher temperatures while sustaining performance and durability. As part of these efforts, high temperature polymer matrix composites and fabrication technologies are being developed for the primary load bearing structure (heat shield) of the spacecraft. New high-temperature resins and composite material manufacturing techniques are available that have the potential to significantly improve current aeroshell design. In order to qualify a polymer matrix composite (PMC) material as a candidate aeroshell structural material, its performance must be evaluated under realistic environments. Thus, verification testing of lightweight PMC's at aeroshell entry temperatures is needed to ensure that they will perform successfully in high-temperature environments. Towards this end, a test program was developed to characterize the mechanical properties of two candidate material systems, T650-35/AFR-PE-4 and T650-35/RP46. The two candidate high-temperature polyimide resins, AFR-PE-4 and RP46, were developed at the Air Force Research Laboratory and NASA Langley Research Center, respectively. This paper presents experimental methods, strength, and stiffness data of the T650-35/AFR-PE-4 material as a function of elevated temperatures. The properties determined during the research test program herein, included tensile strength, tensile stiffness, Poisson s ratio, compressive strength, compressive stiffness, shear modulus, and shear strength. Unidirectional laminates, a cross-ply laminate and two eight-harness satin (8HS)-weave laminates (4-ply and 10-ply) were tested according to ASTM standard methods at room and elevated temperatures (23, 316, and 343 C). All of the relevant test methods and data reduction schemes are outlined along with mechanical data. These data contribute to a database of material properties for high-temperature polyimide composites that will be used to identify the material characteristics of potential candidate materials for aeroshell structure applications.

Whitley, Karen S.↗
NASA NTRS2007

Use of Ionic Liquids in Rod-Coil Block Copolyimides for Improved Lithium Ion Conduction

Solvent-free, solid polymer electrolytes (SPE) have the potential to improve safety, increase design flexibility and enhance performance of rechargeable lithium batteries. Solution based electrolytes are flammable and typically incompatible with lithium metal anodes, limiting energy density. We have previously demonstrated use of polyimide rod coil block copolymers doped with lithium salts as electrolytes for lithium polymer batteries. The polyimide rod blocks provide dimensional stability while the polyethylene oxide (PEO) coil portions conduct ions. Phase separation of the rods and coils in these highly branched polymers provide channels with an order of magnitude improvement in lithium conduction over polyethylene oxide itself at room temperature. In addition, the polymers have been demonstrated in coin cells to be compatible with lithium metal. For practical use at room temperature and below, however, at least an order of magnitude improvement in ion conduction is still required. The addition of nonvolatile, room temperature ionic liquids has been shown to improve the ionic conductivity of high molecular weight PEO. Herein we describe use of these molten salts to improve ionic conductivity in the rod-coil block copolymers.

Meador, Mary Ann B.↗
NASA NTRS2007

Sample mounts for microcrystal crystallography

Sample mounts (10) for mounting microcrystals of biological macromolecules for X-ray crystallography are prepared by using patterned thin polyimide films (12) that have curvature imparted thereto, for example, by being attached to a curved outer surface of a small metal rod (16). The patterned film (12) preferably includes a tapered tip end (24) for holding a crystal. Preferably, a small sample aperture is disposed in the film for reception of the crystal. A second, larger aperture can also be provided that is connected to the sample aperture by a drainage channel, allowing removal of excess liquid and easier manipulation in viscous solutions. The curvature imparted to the film (12) increases the film's rigidity and allows a convenient scoop-like action for retrieving crystals. The polyimide contributes minimally to background and absorption, and can be treated to obtain desired hydrophobicity or hydrophilicity.

Thorne, Robert E.↗