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At least 919 records · Page 51

Development of Processable PMR-Type Polymides with Star-Branched Structures

In the last two decades, high temperature polyimide matrix composites have found broad applications in aerospace structural components, due to their high specific modulus and high specific strength. As matrix resins, aromatic polyimides exhibit exceptional thermal stability and mechanical properties. However, their rodlike structures often result in poor solubility in most common organic solvents, as well as high melt temperature and melt viscosity, making them difficult to process. To overcome this difficulty, flexible linkages including O, SO2 or CH2 non coplanar biphenyl moieties, bulky lateral substituents, and crankshaft structures are often incorporated into the polymer backbones. Addition-curing of low molecular weight polyimides (resins) is another approach to improve processability. One of the most successfully developed materials has been PMR-15 (Polymerization of Monomer Reactants, molecular weight of 1500 g/mol), because of its good combination of thermal and mechanical properties and ease of processability. However, due to the high melt viscosity of PMR-type resins, use of more economical processing methods, such as resin transfer molding (RTM), is not possible. Recent research has focused on the incorporation of trifunctional monomers into addition-curing polyimides in an attempt to improve the processability of these polymers. The objective of this research is to use an aromatic triamine, 1,3,5 tris (4-aminophenoxy) benzene, to prepare new resin systems with starbranched structures. The glass transition temperatures (Tg's) and thermal oxidative stability TOS) of these polymers are compared to their linear counterparts and PMR-15.

Nguyen, Baochau N.↗

Fresnel Concentrators for Space Solar Power and Solar Thermal Propulsion

Large deployable Fresnel concentrators are applicable to solar thermal propulsion and multiple space solar power generation concepts. These concentrators can be used with thermophotovoltaic, solar thermionic, and solar dynamic conversion systems. Thin polyimide Fresnel lenses and reflectors can provide tailored flux distribution and concentration ratios matched to receiver requirements. Thin, preformed polyimide film structure components assembled into support structures for Fresnel concentrators provide the capability to produce large inflation-deployed concentrator assemblies. The polyimide film is resistant to the space environment and allows large lightweight assemblies to be fabricated that can be compactly stowed for launch. This work addressed design and fabrication of lightweight polyimide film Fresnel concentrators, alternate materials evaluation, and data management functions for space solar power concepts, architectures, and supporting technology development.

Bradford, Rodney↗

Preparation and Characterization of Space Durable Polymer Nanocomposite Films from Functionalized Carbon Nanotubes

Low color, flexible, space durable polyimide films with inherent, robust electrical conductivity have been under investigation as part of a continuing materials development activity for future NASA space missions involving Gossamer structures. Electrical conductivity is needed in these films to dissipate electrostatic charge build-up that occurs due to the orbital environment. One method of imparting conductivity is through the use of single walled carbon nanotubes (SWNTs). However, the incompatibility and insolubility of the SWNTs severely hampers their dispersion in polymeric matrices. In an attempt to improve their dispersability, SWNTs were functionalized by the reaction with an alkyl hydrazone. After this functionalization, the SWNTs were soluble in select solvents and dispersed more readily in the polymer matrix. The functionalized SWNTs were characterized by Raman spectroscopy and thermogravimetric analysis (TGA). The functionalized nanotubes were dispersed in the bulk of the films using a solution technique. The functionalized nanotubes were also applied to the surface of polyimide films using a spray coating technique. The resultant polyimide nanocomposite films were evaluated for nanotube dispersion, electrical conductivity, mechanical, and optical properties and compared with previously prepared polyimide-SWNT samples to assess the effects of SWNT functionalization.

Delozier, D. M.↗

The Influence of Sizings on the Durability of High-Temperature Polymer Composites

To increase performance and durability of high-temperature composites for potential rocket engine components, it is necessary to optimize wetting and interfacial bonding between high modulus carbon fibers and high-temperature polyimide resins. Sizings commercially supplied on most carbon fibers are not compatible with polyimides. In this study, the chemistry of sizings on two high-modulus carbon fibers (M40J and M60J, Toray) was characterized as was the chemistry of PMR-II-50 fluorinated polyimide resin. The carbon fibers were characterized using single filament wetting, scanning electron microscopy, fourier transform infrared spectroscopy, and x-ray photoelectron spectroscopic measurements. The polyimide matrix resins were coated onto glass filaments for characterization by wetting measurements. Surface energy components were obtained by wetting with nondispersive (methylene iodide), acidic (ethylene glycol), and basic (formamide) probes. A continuous desizing 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 better bonded composite displayed a tendency to delaminate, presumably due to trapping of volatiles.

Allred, Ronald E.↗

High T(sub g) Polymides for Resin Transfer Molding

A series of new polyimide resins with low melt viscosities and high glass transition temperatures (T(sub g)'s) of 340-350 C were developed for resin transfer molding (RTM) applications. The viscosities of these polyimide resins, based on 2,3,3'4'-Biphenyltetracarboxylic Dianhydride (a-BPDA), are in the range of 10-30 poise. The composites were fabricated successfully at 260-280 C with a pot life of 30-60 minutes by the 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.↗

Mechanically Resilient Polymeric Films Doped with a Lithium Compound

This invention is a series of mechanically resilient polymeric films, comprising rod-coil block polyimide copolymers, which are doped with a lithium compound providing lithium ion conductivity, that are easy to fabricate into mechanically resilient films with acceptable ionic or protonic conductivity at a variety of temperatures. The copolymers consists of short-rigid polyimide rod segments alternating with polyether coil segments. The rods and coil segments can be linear, branched or mixtures of linear and branched segments. The highly incompatible rods and coil segments phase separate, providing nanoscale channels for ion conduction. The polyimide segments provide dimensional and mechanical stability and can be functionalized in a number of ways to provide specialized functions for a given application. These rod-coil black polyimide copolymers are particularly useful in the preparation of ion conductive membranes for use in the manufacture of fuel cells and lithium based polymer batteries.

Mary Ann B Meador↗

Manufacturing Large Membrane Mirrors at Low Cost

Relatively inexpensive processes have been developed for manufacturing lightweight, wide-aperture mirrors that consist mainly of reflectively coated, edge-supported polyimide membranes. The polyimide and other materials in these mirrors can withstand the environment of outer space, and the mirrors have other characteristics that make them attractive for use on Earth as well as in outer space: With respect to the smoothness of their surfaces and the accuracy with which they retain their shapes, these mirrors approach the optical quality of heavier, more expensive conventional mirrors. Unlike conventional mirrors, these mirrors can be stowed compactly and later deployed to their full sizes. In typical cases, deployment would be effected by inflation. Potential terrestrial and outer-space applications for these mirrors include large astronomical telescopes, solar concentrators for generating electric power and thermal power, and microwave reflectors for communication, radar, and short-distance transmission of electric power. The relatively low cost of manufacturing these mirrors stems, in part, from the use of inexpensive tooling. Unlike in the manufacture of conventional mirrors, there is no need for mandrels or molds that have highly precise surface figures and highly polished surfaces. The surface smoothness is an inherent property of a polyimide film. The shaped area of the film is never placed in contact with a mold or mandrel surface: Instead the shape of a mirror is determined by a combination of (1) the shape of a fixture that holds the film around its edge and (2) control of manufacturing- process parameters. In a demonstration of this manufacturing concept, spherical mirrors having aperture diameters of 0.5 and 1.0 m were fabricated from polyimide films having thicknesses ranging from <20 m to 150 m. These mirrors have been found to maintain their preformed shapes following deployment.

FROM↗

Two-Band, Low-Loss Microwave Window

A window for a high-sensitivity microwave receiving system allows microwave radiation to pass through to a cryogenically cooled microwave feed system in a vacuum chamber, while keeping ambient air out of the chamber and helping to keep the interior of the chamber cold. The microwave feed system comprises a feed horn and a low-noise amplifier, both of which are required to be cooled to a temperature of 15 K during operation. The window is designed to exhibit very little microwave attenuation in two frequency bands: 8 to 9 GHz and 30 to 40 GHz. The window is 15 cm in diameter. It includes three layers (see figure): 1) The outer layer is made of a poly(tetrafluoroethylene) film 0.025 mm thick. This layer serves primarily to reflect and absorb solar ultraviolet radiation to prolong the life of the underlying main window layer, which is made of a polyimide that becomes weakened when exposed to ultraviolet. The poly(tetrafluoroethylene) layer also protects the main window layer against abrasion. Moreover, the inherent hydrophobicity of poly(tetrafluoroethylene) helps to prevent the highly undesirable accumulation of water on the outer surface. 2) The polyimide main window layer is 0.08 mm thick. This layer provides the vacuum seal for the window. 3) A 20-mm-thick layer of ethylene/ propylene copolymer foam underlies the main polyimide window layer. This foam layer acts partly as a thermal insulator: it limits radiational heating of the microwave feed horn and, concomitantly, limits radiational cooling of the window. This layer has high compressive strength and provides some mechanical support for the main window layer, reducing the strength required of the main window layer. The ethylene/propylene copolymer foam layer is attached to an aluminum window ring by means of epoxy. The outer poly(tetrafluoroethylene) film and the main polyimide window layer are sandwiched together and pressed against the window ring by use of a bolted clamp ring. The window has been found to introduce a microwave loss of only about 0.4 percent. The contribution of the window to the noise temperature of the microwave feed system has been found to be less than 1 K at 32 GHz and 0.2 K at 8.4 GHz.

Britcliffe, Michael↗

Copoly(Imide Siloxane) Abhesive Materials with Varied Siloxane Oligomer Length

Incorporation of PDMS moieties into a polyimide matrix lowered the surface energy resulting in enhanced adhesive interactions. Polyimide siloxane materials were generated using amine-terminated PDMS oligomers of different lengths to study changes in surface migration behavior, phase segregation, mechanical, thermal, and optical properties. These materials were characterized using contact angle goniometry, tensile testing, and differential scanning calorimetry. The surface migration behavior of the PDMS component depended upon the siloxane molecular weight as indicated by distinct relationships between PDMS chain length and advancing water contact angles. Similar correlations were observed for percent elongation values obtained from tensile testing, while the addition of PDMS reduced the modulus. High fidelity topographical modification via laser ablation patterning further reduced the polyimide siloxane surface energy. Initial particulate adhesion testing experiments demonstrated that polyimide siloxane materials exhibited greater abhesive interactions relative to their respective homopolyimides.

Wohl, Christopher J.↗

Blocking Filters with Enhanced Throughput for X-Ray Microcalorimetry

New and improved blocking filters (see figure) have been developed for microcalorimeters on several mission payloads, made of high-transmission polyimide support mesh, that can replace the nickel mesh used in previous blocking filter flight designs. To realize the resolution and signal sensitivity of today s x-ray microcalorimeters, significant improvements in the blocking filter stack are needed. Using high-transmission polyimide support mesh, it is possible to improve overall throughput on a typical microcalorimeter such as Suzaku s X-ray Spectrometer by 11%, compared to previous flight designs. Using polyimide to replace standard metal mesh means the mesh will be transparent to energies 3 keV and higher. Incorporating polyimide s advantageous strength-to-weight ratio, thermal stability, and transmission characteristics permits thinner filter materials, significantly enhancing through - put. A prototype contamination blocking filter for ASTRO-H has passed QT-level acoustic testing. Resistive traces can also be incorporated to provide decontamination capability to actively restore filter performance in orbit.

Grove, David↗

Space Shuttle Columbia Aging Wiring Failure Analysis

A Space Shuttle Columbia main engine controller 14 AWG wire short circuited during the launch of STS-93. Post-flight examination divulged that the wire had electrically arced against the head of a nearby bolt. More extensive inspection revealed additional damage to the subject wire, and to other wires as well from the mid-body of Columbia. The shorted wire was to have been constructed from nickel-plated copper conductors surrounded by the polyimide insulation Kapton, top-coated with an aromatic polyimide resin. The wires were analyzed via scanning electron microscope (SEM), energy dispersive X-Ray spectroscopy (EDX), and electron spectroscopy for chemical analysis (ESCA); differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) were performed on the polyimide. Exemplar testing under laboratory conditions was performed to replicate the mechanical damage characteristics evident on the failed wires. The exemplar testing included a step test, where, as the name implies, a person stepped on a simulated wire bundle that rested upon a bolt head. Likewise, a shear test that forced a bolt head and a torque tip against a wire was performed to attempt to damage the insulation and conductor. Additionally, a vibration test was performed to determine if a wire bundle would abrade when vibrated against the head of a bolt. Also, an abrasion test was undertaken to determine if the polyimide of the wire could be damaged by rubbing against convolex helical tubing. Finally, an impact test was performed to ascertain if the use of the tubing would protect the wire from the strike of a foreign object.

McDaniels, Steven J.↗

Thermally-rearranged polymer blends for gas separation membranes

Polymer blends comprising an ortho-functionalized polyimide homo or copolymer and a polybenzimidazole homo or copolymer, wherein the ortho-functionalized polyimide thermally rearranges to a polymer comprising a phenylene heterocyclic group, such as, polybenzoxazole, polybenzothiazole, polybenzimidazole and/or other heterocyclic structure upon heating. Also disclosed are method of forming a polymer blend comprising dissolving an ortho-functionalized polyimide homo or copolymer and a polybenzimidazole homo or copolymer in a solvent, and optional compatibilizer, to form a polymer solution; contacting a support with the polymer solution; and evaporating the solvent to provide a thin layer comprising the polymer blend on the support. Further, methods of heat treating these polymer blends to thermally rearrange the disclosed polyimides are disclosed, as are the polymer blends prepared thereby. Methods of using these polymer blends to separate gases are also disclosed.

Freeman, Benny D.↗

Ultra-low radioactivity flexible printed cables

Abstract Flexible printed cables and circuitry based on copper-polyimide materials are widely used in experiments looking for rare events due to their unique electrical and mechanical characteristics. However, past studies have found copper-polyimide flexible cables to contain 400-4700 pg 238 U/g, 16-3700 pg 232 Th/g, and 170-2100 ng nat K/g, which can be a significant source of radioactive background for many current and next-generation ultralow background detectors. This study presents a comprehensive investigation into the fabrication process of copper-polyimide flexible cables and the development of custom low radioactivity cables for use in rare-event physics applications. A methodical step-by-step approach was developed and informed by ultrasensitive assay to determine the radiopurity in the starting materials and identify the contaminating production steps in the cable fabrication process. Radiopure material alternatives were identified, and cleaner production processes and treatments were developed to significantly reduce the imparted contamination. Through the newly developed radiopure fabrication process, fully-functioning cables were produced with radiocontaminant concentrations of 20-31 pg 238 U/g, 12-13 pg 232 Th/g, and 40-550 ng nat K/g, which is significantly cleaner than cables from previous work and sufficiently radiopure for current and next-generation detectors. This approach, employing witness samples to investigate each step of the fabrication process, can hopefully serve as a template for investigating radiocontaminants in other material production processes.

36 MATERIALS SCIENCE↗

Approaching air buoyancy in aero/cryogel vacuum vessels

Air impermeability has been observed in low-density aerogel and cryogel materials, which has led to a series of experiments to investigate the feasibility of an air buoyant vacuum vessel, as well as the fabrication and testing of sub-buoyant prototypes. Here, bulk samples of silica aerogel were shown to isolate vacuum from ambient air for several hours with optimal vacuum isolation occurring at a density of approximately 85 mg cm –3 . It was demonstrated using polyimide aerogel and cryogel materials that the ability of these foam materials to provide an air impermeable layer between vacuum and atmosphere, in spite of being comprised of mostly void space, is related to material stiffness. It is hypothesized that this behavior is due to local deformation of the random nanostructure of the material. Spherical shell vacuum vessels were produced using the polyimide cryogel, and less than 133 Pa vacuum containment was demonstrated under active pumping. In order to approach the non-buoyant to buoyant transition for these vacuum vessels, a polyimide composite was produced using helical fibers for which preliminary mechanical testing was performed.

36 MATERIALS SCIENCE↗

Material erosion measurements and expected operational lifetime of a deployable photon sieve payload

Spacecraft operating in low-Earth orbit are subjected to a number of hazardous environmental constituents that can lead to decreased system performance and reduced operational lifetimes. Due to their thermal, optical, and mechanical properties, polymers are used extensively in space systems; however they are particularly susceptible to material erosion and degradation as a result of exposure to the LEO environment. The focus of this research is to examine the material erosion and mass loss experienced by a custom Kaptonlike polyimide due to exposure in a simulated low-earth orbit environment. The deployable membrane telescope design discussed in this research is named Peregrine and is the scientific payload for FalconSat-7, a 3U cubesat designed and developed at the United States Air Force Academy (USAFA) for the purpose of demonstrating the capability of deployable membrane telescope technology on a nanosatellite platform. In addition to the polymer samples, chrome, silver and gold specimens will be examined to measure the oxidation rate and act as a control specimen, respectively. A magnetically filtered atomic oxygen plasma source has previously been developed and characterized for the purpose of simulating the low-Earth orbit environment. The plasma source can be operated at a variety of discharge currents and gas flow rates, of which the plasma parameters downstream of the source are dependent. The characteristics of the generated plasma were examined as a function of these operating parameters to optimize the production of O + ions with energy relevant to LEO applications. The erosion yield of the Kapton-like polyimide was experimentally determined to be 2.84 x 10 -24 cm 3 per atom which is in close agreement when compared to the on-orbit measurement for reaction efficiency of Kapton HN. We report the experimentally determined reaction rate for the Kapton-like polyimide was used to estimate the operational lifetime of the photon sieve during the solar conditions expected beginning in May 2019. The effective lifetime is estimated between 126 and 153 days.

36 MATERIALS SCIENCE↗

Multimaterial Aerosol Jet Printed Magnetic Nanocomposites for Microwave Circuits

Here this article demonstrates the process and characterization of additively manufactured polymer-matrix magnetic nanocomposites. These nanocomposites are composed of nickel-zinc ferrite (Ni 0.5 Zn 0.5 Fe 2 O 4 ) nanoparticles in a polyimide matrix. These materials are printed using multimaterial aerosol jet printing where aerosols of nickel-zinc ferrite and polyimide inks are mixed in place to fabricate structures with nonunity relative permeability. To characterize these materials, we use energy-dispersive X-ray spectroscopy to estimate the content of ferrite in the composite, fitted simulation models, and ring resonator measurements to estimate the permeability. In fully aerosol jet printed 1-mm 2 inductors, we demonstrate an increase in inductance density of 40% in a 4.5-turn microstrip spiral inductor using this printed composite. These fully printed inductors demonstrate an inductance density of 4.2-nH/mm 2 . EDS analysis shows films with 18 wt.% Ni 0.5 Zn 0.5 Fe 2 O 4 . Finally, we show microstrip transmission lines on printed composite compared to the same on polyimide subjected to a dc magnetic bias, displaying a magnetic resonance behavior.

42 ENGINEERING↗

Cryogenic/high temperature structural adhesives

Results are described of the work performed to develop a structural adhesive system which possesses useful properties over a 20K (-423 F) to 589 K (600 F) temperature range. Adhesives systems based on polyimide, polyphenylquinoxaline polyquinoxaline, polybenzothiazole and polybenzimidazole polymers first were screened for suitability. Detailed evaluation of two polyimide adhesive sytems, Br34/FM34 and P4/A5F or P4A/A5FA, and one polyphenylquinoxaline adhesive system, PPQ II (IMW), then was performed. Property information was generated over the full temperature range for shear strength, stressed and unstressed thermal aging, thermal shock and coefficient of thermal expansion. Both polyimide adhesive systems were identified as being capable of providing structural adhesive joints for cryogenic/high temperature service.

Vaughan, R. W.↗

Evaluation of polyimide/glass fiber composites for construction of light weight pressure vessels for cryogenic propellants

The application of polyimide resin as a matrix for glass filament-wound thin metal-lined pressure vessels was studied over a temperature range of (minus) 320 to 600 F. Keramid 601 polyimide was found to perform quite well over the entire range of temperature. Hoop stress values of 425 ksi were determined at 75 F which is equivalent to epoxy resin in similar structures. At -320 and 600 F, 125 and 80% of this strength was retained. Thermal ageing at 500 F for up to 50 hours was studied with severe reduction in strength, but there is evidence that this reduction could be improved. Another polyimide resin studied was P10PA which was found to have processing characteristics inappropriate for filament-winding. NOL ring tensile and shear data was determined from both resins with S-glass. Pressure vessel design, fabrication and test procedures are described in detail.

Petker, I.↗