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The failure surface analysis of adhesively bonded carbon fiber composites is described. The emphasis is on the bonding of composites when the surface has been made intentionally resin-rich. Also discussed is surface analysis of both commercially available and pretreated carbon fibers. The interaction of the fibers with polysulfone is described.
A study is presented of the effect of radiation on polymers. It helps to estimate the impact of the space environment on composite structures. Two commercially available polymer films were used; a polyetherimide, and a polysulfone. Both films were irradiated in vacuum with 85 KeV electron. Properties of the films before and after irradiation were monitored by tensile elongation measurements, ultraviolet/visible spectroscopy, glass transition temperature measurements, gel permeation chromatography, and infrared spectroscopy. The results of these characterizations are presented and briefly discussed.
Amine functional poly(arylene ether) sulfones were previously reported. Herein, the chemistry was extended to amorphous poly(arylene ether) ketones because of their higher fracture toughness values, relative to the polysulfones. It was demonstrated that the amino functional oligomers undergo a self-crosslinking reaction at temperatures above about 220 C. This produces an insoluble, but ductile network that has excellent resistance. A ketamine structure hypothesis was proposed and verified using solid state magic angle NMR. In most cases, the water generated upon ketamine formation is too low to produce porosity and solid networks are obtained. The stability of the ketamine networks towards hydrolysis is excellent. The chemistry was further demonstrated to be able to crosslink preformed nonfunctional poly(arylene ether) ketones if a difunctional amine was utilized. This concept has the possibility of greatly improving the creep resistance of thermoplastics. Also, a new technique was developed for converting the amine functional oligomers cleanly into maleimide structures. This method involves reacting maleic anhydride with monomeric aminophenols in the presence of solvent mixtures.
Relative adhesion strengths between AS4, AS1, and XAS carbon fibers and thermoplastic polymers were determined using the embedded single filament test. Polymers studied included polycarbonate, polyphenylene oxide, polyetherimide, polysulfone, polyphenylene oxide blends with polystyrene, and polycarbonate blends with a polycarbonate polysiloxane block copolymer. Fiber surface treatments and sizings improved adhesion somewhat, but adhesion remained well below levels obtained with epoxy matrices. An explanation for the differences between the Hercules and Grafil fibers was sought using X ray photon spectroscopy, wetting, scanning electron microscopy and thermal desorption analysis.
Results are reported from a study of the stability of poly(arylene ethers) formed in a reaction of 1,3 -bis(4-chlorobenzoyl)benzene and various bisphenols after experiencing long-term exposure to space conditions. Transparent poly(arylene ethers) films were subjected to separate electron and UV bombardments, as were polysulfone and Kapton films for comparisons. The order of exposure to the two types of radiation was reversed for two sample populations. The optical properties and glass transition temperatures of the samples were determined after irradiation. The poly(arylene ethers) films exhibited good resistance to the electron radiation but suffered severe degradation in the UV environment. The loss of optical transmissivity was proportional to the UV radiation dose.
In a continuing effort to synthesize polymers that are readily processable and that exhibit state-of-the-art characteristics, LARC-TPI (Mitsui) and polyimidesulfone (PISO2) were blended and subjected to a limited melt flow and thermal properties characterization. Mitsui Toatsu of Japan, working under a licensing agreement with NASA, synthesized an imidized version of LARC-TPI molding powder that exhibited an extraordinarily high level of softening when heated to 300 C. Subsequently, a study of the calorimetric and rheological properties was accomplished by NASA-Langley on that material. The thermoplastic polyimidesulfone that possesses processability similar to polysulfones and the solvent resistance of the polyimides was synthesized and characterized at NASA-Langley in the early 1980's.
An evaluation has been undertaken of blends of a novel ethynyl-terminated imidothioether with Udel P1700 polysulfone and ethynyl-terminated arylene ether oligomers. Good to excellent processability was obtained with these blends using compression molding; the cured blends displayed poor-to-good resistance to chloroform and low-to-moderately high fracture toughness, depending on the blends' crosslink density. The flexural strength and modulus of unidirectional carbon graphite laminates prepared with the blended resins were good.
It is important to study changes in properties of polymeres after irradiation with charged particles, with ultraviolet radiation, and with combinations of both. An apparatus for this purpose has been built at the NASA Langley Research Center. It consists of a chamber 9 inches in diameter and 9 inches high with a port for an electron gun, another port for a mass spectrometer, and a quartz window through which an ultraviolet lamp can be focused. The chamber, including the electron gun and the mass spectrometer, can be evacuated to a pressure of 10 to the 8th power torr. A sample placed in the chamber can be irradiated with electrons and ultraviolet radiation separately, sequentially, or simultaneously, while volatile products can be monitored during all irradiations with the mass spectrometer. The apparatus described above has been used to study three different polymer films: lexan; a polycarbonate; P1700, a polysulfone; and mylar, a polyethylene terephthalate. All three polymers had been studied extensively with both electrons and ultraviolet radiation separately, but not simultaneously. Also, volatile products had not been monitored during irradiation for the materials. A high electron dose rate of 530 Mrads/hr was used so that a sufficient concentration of volatile products would be formed to yield a reasonable mass spectrum.
At the altitudes of low-earth orbit (LEO), atomic oxygen (AO) is the most abundant chemical species. This strong oxidizing agent reacts with virtually any organic material that is not already fully oxidized. Erosion by AO can be extensive and jeopardizes any protective coatings, thermal blankets, adhesives, and structural composites exposed on the exterior of satellites in LEO. Researchers prepared and tested organic materials for their susceptibility to AO using a commercial plasma asher which approximately simulates the oxygen effects in LEO. Experiments were performed on a polyimide, a polysulfone, and two epoxy adhesives into which low molecular-weight additives have been dissolved. Incorporated in the molecular structure of these additives are elements such as silicon whose nonvolatile oxides, which are formed on exposure to AO, remain as a coating on the surface to create a barrier between the remainder of the organic material and the AO. We find that the additives protect the materials, but the low solubility of some limit their utility. Concurrent studies are underway to measure the effect of the additives on the thermal expansion coefficients of the materials. Tows of aramid fibers, which are important components in the proposed tether satellite systems, have been eroded in the asher. The results which show that the square root of the mass remaining decreases linearly with the time of exposure (see the figure) are consistent with a constant rate of surface erosion. The tensile strength of these eroded tows decreases with time of exposure also; additional measurements are in progress.
A microgravity whole body shower (WBS) and waste water recovery systems (WWRS) were evaluated in three separate closed loop tests. Following a protocol similar to that anticipated for the U.S. Space Station, test subjects showered in a prototype whole body shower. The WWRS processes evaluated during the test series were phase change and reverse osmosis (RO). A preprototype Thermoelectric Integrated Hollow Fiber Membrane Evaporation Subsystem phase change process was used for the initial test with chemical pretreatment of the shower water waste input. The second and third tests concentrated on RO technologies. The second test evaluated a dynamic RO membrane consisting of zirconium oxide polyacrylic acid (ZOPA) membranes deposited on the interior diameter of 316L porous stainless steel tubes while the final test employed a thin semipermeable RO membrane deposited on the interior surface of polysulfone hollow fibers. All reclaimed water was post-treated for purity using ion exchange and granular activated carbon beds immediately followed by microbial control treatment using both heat and iodine. The test hardware, controls exercised for whole body showering, types of soaps evaluated, shower subject response to reclaimed water showering, and shower water collection and chemical pretreatment (if required) for microbial control are described. The WWRS recovered water performance and the effectiveness of the reclaimed water post-treatment techniques used for maintaining water purity and microorganism control are compared. Results on chemical and microbial impurity content of the water samples obtained from various locations in the shower water reuse system are summarized.
Summarized are basic studies that were conducted to correlate the impact resistance of graphite-fiber-reinforced composites with polymer matrix properties. Three crosslinked epoxy resins and a linear polysulfone were selected as composite matrices. As a group, these resins possess a significantly large range of mechanical properties. The mechanical properties of the resins and their respective composites were measured. Neat resin specimens and unidirectional and crossply composite specimens were impact tested with an instrumented dropweight tester. Impact resistances of the specimens were assesseed on the basis of loading capability, energy absorption, and extent of damage.
Thin layer of polysulfone on polycarbonate safety helmets and visors protects them from attack by chemicals. Useful in industrial safety helmets. Highly resistant to creep under tension load. Retains dimensional stability when exposed to moisture. Does not adversely affect optical properties of polycarbonate visors. Configuration varied to accommodate such special requirements as high impact strength or protection against moving particles and debris.
The synthesis of polymers is discussed. It includes: (1) the synthesis of fluorine-containing crosslinked poly(ether ketones); (2) the synthesis and characterization of poly(imide amides) and their N-methylated analogues; (3) the synthesis of fluorine-containing aromatic polyethers; (4) the synthesis of novel fluorine-containing aromatic polysiloxanes; and (5) the conversion of 6F-containing polythioethers to polysulfones. It is hoped that these polymers will find use as low dielectric materials in electronic applications, function as thermal control coatings, or be suitable elastomeric sealants for extreme service conditions.
The adhesion strength of AS4 fibers to thermoplastic polymers was determined. The specific polymers were polycarbonate, polyphenylene oxide, polyetherimide, polyphenylene oxide blends with polystyrene, and polycarbonate blends with a polycarbonate-polysiloxan copolymer. Data are also included for polysulfone. It was recognized at the outset that an absolute measure of the fiber matrix adhesion would be difficult. However, it is feasible to determine the fiber bond strengths to the thermoplastics relative to the bond strengths of the same fibers to epoxy polymers. It was anticipated, and in fact realized, that the adhesion of AS4 to the thermoplastic polymers was relatively low. Therefore, further objectives of the study were to identify means of increasing fiber/matrix adhesion and to try to determine why the adhesion of AS4 to thermoplastics is significantly less than to epoxy polymers.
Chemical characterization of selected polymeric materials which received exposure on the Long Duration Exposure Facility (LDEF) is reported. The specimens examined include silvered fluorinated ethylene propylene Teflon thermal blanket material, polysulfone, epoxy, polyimide matrix resin/graphite fiber reinforced composites, and several high performance polymer films. These specimens came from numerous LDEF locations, and thus received different environmental exposures. The results to date show no significant change at the molecular level in the polymer that survived exposure. Scanning electron and scanning tunneling microscopes show resin loss and a texturing of some specimens which resulted in a change in optical properties. The potential effect of a silicon-containing molecular contamination on these materials is addressed. The possibility of continued post-exposure degradation of some polymeric films is also proposed.
The Advanced composites Sub-experiment includes numerous metal matrix composites, primarily graphite fiber reinforced aluminum and magnesium, and several classes of graphite fiber reinforced organic matrix (epoxy, polysulfone, polyimide) composites with and/or without thermal control or protective coatings. The experiment included over 500 flight samples, mounted on the leading and trailing edges of LDEF, and a full complement of the laboratory control samples. Preliminary results are presented reviewing changes in the visual appearance of the samples, atomic oxygen erosion of the organic matrix composites, contamination effects, and the effects of micrometeorite impacts and thermal fatigue on the metal matrix composites.
The characterization of selected graphite fiber reinforced epoxy and polysulfone matrix resin composites which received exposure to the LEO environment on the LDEF is reported. The changes in mechanical properties of ultimate tensile strength and tensile modulus for exposed flight specimens are compared to the three sets of control specimens. Marked changes in surface appearance are discussed, and resin loss is reported. The chemical characterization including IR, thermal, and selected solution property measurements showed that the molecular structure of the polymeric matrix had not changed significantly in response to this exposure.
The chemical characterization of selected polymeric materials which received exposure on the LDEF is reported. The specimens examined include silvered fluorinated ethylene propylene (FEP) teflon thermal blanket material, polysulfone matrix resin/graphite fiber reinforced composites, and several high performance polymer films. These specimens came from numerous LDEF locations and, thus, received different environmental exposures. The results of infrared, thermal, x ray photoelectron, and various solution property analyses have shown no significant change at the molecular level in the polymer that survived exposure. However, scanning electron and scanning tunneling microscopies show resin loss and a texturing of the surface of some specimens which resulted in a change in optical properties. The potential effect of a silicon containing molecular contamination on these materials is addressed. The possibility of continued post-exposure degradation of some polymeric films is also proposed.