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NASA NTRS2021

Thermal Conductivity Estimation from Transient Test Data with Embedded Thermocouples using Genetic Algorithm Optimization

Inverse heat transfer methodology previously developed to estimate thermal properties of high temperature fibrous insulation from embedded thermocouples was applied to the thermoplastic polymer, polyether-ether-ketone (PEEK). A small experimental setup was utilized to test the PEEK sample between temperatures of 300 K and 525 K at atmospheric pressure. Cylindrical plugs of PEEK with three thermocouples embedded at various depths were incorporated in the test sample. The experimental PEEK thermocouple data were used as the boundary and initial conditions of a one-dimensional numerical thermal model to predict the internal temperatures of the material. The thermal conductivity of PEEK was estimated with the Continuous Genetic Algorithm optimization technique by searching for the coefficients of a functional form of thermal conductivity that minimized the difference between the experimentally measured and model predicted internal temperature values. The thermal testing, one-dimensional numerical thermal model, optimization algorithm, analysis, and results are presented.

Thermal Properties↗
NASA NTRS2024

Additively Manufactured Plastic Plasma Spectrometer

We report results in development and testing of a low resource top hat electrostatic analyzer (ESA) for space plasma measurements. This device has been additively manufactured (3D-printed) using fused deposition modeling. The classic top hat design is composed of four plastic pieces, without any surface coatings. The three conducting electrodes are printed from carbon nanotube infused polyether ether ketone (CNT-PEEK). The fourth piece, an insulating electrode support, uses pure PEEK. This ESA is designed to detect electrons in space from 10eV up to 30 keV. We demonstrate that the printed CNT-PEEK is sufficiently electrically conductive to support the fast high voltage slewing often required for high time resolution measurements. The plastic ESA has been successfully vibrated beyond standard pre-flight levels, tested under keV electron beam illumination over a wide range of temperatures, and tested under UV illumination, simulating the solar Ly-α flux. In comparison with an identical machined aluminum ESA, our CNT-PEEK ESA provides nominal energy/angle band passes, closely matching simulation. These band passes imply minimal impact from surface charging at beam energies of 2-3 keV, although more investigation is needed. We also find that the CNT-PEEK ESA provides far superior out-of-band electron rejection and UV photon rejection compared to the machined aluminum ESA. We do not detect any problems with trapped gases or outgassing. This development offers potential for significant mass savings, implementation of otherwise unattainable geometric configurations, and dramatic simplification in manufacturing and assembly processes required for development of space plasma instruments.

Quetzal Larrick↗
NASA NTRS1988

The crystallization of tough thermoplastic resins in the presence of carbon fibers

The presence of carbon fibers increased the crystallization rates of both PEEK and PPS thermoplastic polymers. The effect was most pronounced at higher crystallization temperatures. Isothermal crystallization rates were analyzed by applying classical phenomenological nucleation theory. Unusually high values of the so-called Avrami exponent were found for neat PEEK. Isothermal crystallization of PEEK and PPS polymers produced crystalline samples having a wide variety of melting temperatures. The melting as observed by differential scanning calorimetry occurred as dual endotherms which were called primary (higher temperature) and secondary melting peaks. Each primary peak accounted for most of the crystallinity present. The secondary peaks represented the melting of crystallites formed later than those attributable to the primary endotherms. The presence of carbon fibers increased the thermal stability of both PEEK and PPS crystallites as manifested by higher temperatures for the primary melting peaks. This may be attributable to increased crystallite size, greater crystallite perfection, and/or favorable modification of the crystallite interface. Over the range studied, crystallization temperature strongly influenced the positions of the secondary peaks but not the primary peaks.

Theil, Michael H.↗
NASA NTRS1988

Non-isothermal crystallization of poly(etheretherketone) aromatic polymer composite

The nonisothermal crystallization kinetics of PEEK APC-2 and of 450G neat resin PEEK material were compared using a differential scanning calorimeter to monitor heat flow during crystallization; the effects of cooling rate on the crystallization temperature, the degree of crystallinity, and the conversion rate were investigated. A modified Avrami (1940) analysis was used to describe nonisothermal crystallization kinetics. It was found that, compared with the 450G neat resin PEEK, the nonisothermal crystallization of the PEEK APC-2 composite is characterized by higher initiation temperature, higher heat flow maximum temperature, and greater relative conversion by primary processes.

Cebe, Peggy↗
NASA NTRS1991

Investigation of microstructural changes in polyetherether-ketone films at cryogenic temperatures by positron lifetime spectroscopy

Microstructural changes in Polyetherether-ketone (PEEK) films were investigated in the temperature ranges of 23 to -196 C, using Positron Lifetime Spectroscopy (PLS) technique. It was determined that the total free volume decreases by about 46 percent in amorphous PEEK samples and about 36 percent in semicrystalline PEEK samples when they are cooled down from room temperature to liquid nitrogen (LN2) temperature. If this trend in reduction in free volume with decreasing temperature continues, as expected, it is surmised that PEEK will be able to withstand cooling down to liquid hydrogen (LH2) temperature without any detrimental effect on its diffusivity for liquid hydrogen.

Singh, Jag J.↗
NASA NTRS1990

Supportability evaluation of thermoplastic and thermoset composites

Nearly 300 advanced composite components manufactured by Northrop Corporation are flying on U.S. Air Force and U.S. Navy supersonic aircraft as part of a three-year Air Force/Navy/Northrop supportability evaluation. Both thermoplastic and high-temperature thermoset composites were evaluated for their in-service performance on 48 USAF and Navy F-5E fighter and USAFT-38 trainer aircraft in the first large-scale, long-term maintenance evaluation of these advanced materials. Northrop manufactured four types of doors for the project-avionics bay access, oil fill, inlet duct inspection, and a main landing gear door. The doors are made of PEEK (polyetheretherketone) thermoplastic, which is tougher and potentially less expensive to manufacture than conventional composites; and 5250-3 BMI (bismaleimide) thermoset, which is manufactured like a conventional epoxy composite but can withstand higher service temperatures. Results obtained so far indicate that both the BMI and PEEK are durable with PEEK being somewhat better than BMI.

Chanani, G. R.↗
NASA NTRS1994

Mechanical property characterization and impact resistance of selected graphite/PEEK composite materials

To use graphite polyetheretherketone (PEEK) material on highly curved surfaces requires that the material be drapable and easily conformable to the surface. This paper presents the mechanical property characterization and impact resistance results for laminates made from two types of graphite/PEEK materials that will conform to a curved surface. These laminates were made from two different material forms. These forms are: (1) a fabric where each yarn is a co-mingled Celion G30-500 3K graphite fiber and PEEK thermoplastic fiber; and (2) an interleaved material of Celion G30-500 3K graphite fabric interleaved with PEEK thermoplastic film. The experimental results from the fabric laminates are compared with results for laminates made from AS4/PEEK unidirectional tape. The results indicate that the tension and compression moduli for quasi-isotropic and orthotropic laminates made from fabric materials are at least 79 percent of the modulus of equivalent laminates made from tape material. The strength of fabric material laminates is at least 80 percent of laminates made from tape material. The evaluation of fabric material for shear stiffness indicates that a tape material laminate could be replaced by a fabric material laminate and still maintain 89 percent of the shear stiffness of the tape material laminate. The notched quasi-isotropic compression panel failure strength is 42 to 46 percent of the unnotched quasi-isotropic laminate strength. Damage area after impact with 20 ft-lbs of impact energy is larger for the co-mingled panels than for the interleaved panels. The inerleaved panels have less damage than panels made from tape material. Residual compression strength of quasi-isotropic panels after impact of 20 ft-lbs of energy varies between 33 percent of the undamaged quasi-isotropic material strength for the tape material and 38 percent of the undamaged quasi-isotropic material strength for the co-mingled fabric material.

Baker, Donald J.↗
NASA NTRS2012

High-Temperature Shape Memory Polymers

physical conformation changes when exposed to an external stimulus, such as a change in temperature. Such materials have a permanent shape, but can be reshaped above a critical temperature and fixed into a temporary shape when cooled under stress to below the critical temperature. When reheated above the critical temperature (Tc, also sometimes called the triggering or switching temperature), the materials revert to the permanent shape. The current innovation involves a chemically treated (sulfonated, carboxylated, phosphonated, or other polar function group), high-temperature, semicrystalline thermoplastic poly(ether ether ketone) (Tg .140 C, Tm = 340 C) mix containing organometallic complexes (Zn++, Li+, or other metal, ammonium, or phosphonium salts), or high-temperature ionic liquids (e.g. hexafluorosilicate salt with 1-propyl-3- methyl imidazolium, Tm = 210 C) to form a network where dipolar or ionic interactions between the polymer and the low-molecular-weight or inorganic compound forms a complex that provides a physical crosslink. Hereafter, these compounds will be referred to as "additives". The polymer is semicrystalline, and the high-melt-point crystals provide a temporary crosslink that acts as a permanent crosslink just so long as the melting temperature is not exceeded. In this example case, the melting point is .340 C, and the shape memory critical temperature is between 150 and 250 C. PEEK is an engineering thermoplastic with a high Young fs modulus, nominally 3.6 GPa. An important aspect of the invention is the control of the PEEK functionalization (in this example, the sulfonation degree), and the thermal properties (i.e. melting point) of the additive, which determines the switching temperature. Because the compound is thermoplastic, it can be formed into the "permanent" shape by conventional plastics processing operations. In addition, the compound may be covalently cross - linked after forming the permanent shape by S-PEEK by applying ionizing radiation ( radiation, neutrons), or by chemical crosslinking to form a covalent permanent network. With respect to other shape memory polymers, this invention is novel in that it describes the use of a thermoplastic composition that can be thermally molded or solution-cast into complex "permanent" shapes, and then reheated or redissolved and recast from solution to prepare another shape. It is also unique in that the shape memory behavior is provided by a non-polymer additive.

Yoonessi, Mitra↗
NASA NTRS1988

Annealing study of poly(etheretherketone)

Annealing of PEEK has been studied for two materials cold-crystallized from the rubbery amorphous state. The first material is a low molecular weight PEEK; the second is commercially available neat resin. Differential scanning calorimetry was used to monitor the melting behavior of annealed samples. The effect of thermal history on melting behavior is very complex and depends upon annealing temperature, residence time at the annealing temperature, and subsequent scanning rate. Thermal stability of both materials is improved by annealing, and for an annealing temperature near the melting point, the polymer can be stabilized against reorganization during the scan. Variations of density, degree of crystallinity, and X-ray long period were studied as a function of annealing temperature for the commercial material.

Cebe, Peggy↗
NASA NTRS1988

Pultrusion with thermoplastics for the fabrication of structures in space

The use of the pultrusion method to produce structures in space is proposed. This technique is based on transporting materials in coils or bundles and fabricating the structures in space. Two methods for thermoplastic impregnation of advanced composite are described. The properties of three pultruded thermoplastic matrix materials, polyphenylene sulfide, polyetherimide (PEI), and polyetheretherketone (PEEK) are discussed and evaluated. It is observed that the pultrusions containing PEI and PEEK reveal post-fabrication potential of lightweight, high strength advanced composites and this method of fabrication produces strength values comparable to those of conventional techniques. Earth-based and space-based planetary shelter models are developed and compared. It is noted that cargo storage volume is dependent on a combination of profiles, packaging, and manufacturing methods.

Wilson, Maywood L.↗
NASA NTRS1989

Electrostatic prepregging of thermoplastic matrices

Thermoplastic towpregs of PEEK/AS-4, PEEK/S-2 glass and LaRC-TPI/AS-4, produced by electrostatic deposition of charged and fluidized polymer powders on spread continuous fiber tows, are described. Processing parameters for combining PEEK 150 powder with unsized 3k AS-4 carbon fiber are presented. The experimental results for PEEK 150/AS-4 reveal that electrostatic fluidized bed coating may be an economically attractive process for producing towpreg.

Muzzy, John D.↗
NASA NTRS1990

Cross-sectional examination of the damage zone in impacted specimens of carbon/epoxy and carbon/PEEK composites

Drop weight impact testing was utilized to inflict damage on eight-ply bidirectional and unidirectional samples of carbon/epoxy and carbon/PEEK (polyetheretherketone) test specimens with impact energies ranging from 0.80 J to 1.76 J. The impacting tip was of a smaller diameter (4.2-mm) than those used in most previous studies, and the specimens were placed with a diamond wheel wafering saw through the impacted area perpendicular to the outer fibers. Photographs at 12 x magnification were taken of these cross-sections and examined. The results on the bidirectional samples show little damage until 1.13 J, at which point delaminations were seen in the epoxy specimens. The PEEK specimens showed less delamination than the epoxy specimens for a given impact energy level. The unidirectional specimens displayed more damage than the bidirectional samples for a given impact energy, with the PEEK specimens showing much less damage than the epoxy material.

Nettles, A. T.↗
NASA NTRS1991

Impact Damage In Carbon/Epoxy And Carbon/PEEK Composites

Report describes results of drop-weight impact testing of specimens of carbon-fiber/epoxy and carbon-fiber/polyetheretherketone (PEEK) composite materials. Panels made of these materials assembled into lightweight, strong, stiff structures useful in automobiles, aircraft, sporting goods, and many other products. PEEK specimens showed less delamination than epoxy specimens at given impact energy.

Nettles, A. T.↗
NASA NTRS1991

Mechanical property characterization and impact resistance of selected graphite/PEEK composite materials

To use graphite/PEEK material on highly curved surfaces requires that the material be drapable and easily conformable to the surface. The mechanical property characterization and impact resistance results are presented for laminates made from two types of graphite/PEEK materials that will conform to a curved surface. These laminates were made from two different material forms. These forms are: (1) a fabric where each yarn is a co-mingled Celion G30-500 3K graphite fiber and PEEK fiber; and (2) an interleaved material of Celion G30-500 3K graphite fiber interleaved with PEEK film. The experimental results from the fabric laminates are compared with results for laminates made from AS4/PEEK unidirectional tape. The results indicate that the tension and compression moduli for quasi-isotropic and orthotropic laminates made from fabric materials are at least 98 pct. of the modulus of equivalent laminates made from tape materials. The strength of fabric material laminates is at least 80 pct. of laminates made from tape material. The evaluation of the fabric material for shear stiffness indicates that a tape material laminate could be replaced by a fabric material laminate and still maintain 89 pct. of the shear stiffness of the tape material laminate.

Baker, Donald J.↗
NASA NTRS1991

Mechanical properties of 2D and 3D braided textile composites

The purpose of this research was to determine the mechanical properties of 2D and 3D braided textile composite materials. Specifically, those designed for tension or shear loading were tested under static loading to failure to investigate the effects of braiding. The overall goal of the work was to provide a structural designer with an idea of how textile composites perform under typical loading conditions. From test results for unnotched tension, it was determined that the 2D is stronger, stiffer, and has higher elongation to failure than the 3D. It was also found that the polyetherether ketone (PEEK) resin system was stronger, stiffer, and had higher elongation at failure than the resin transfer molding (RTM) epoxy. Open hole tension tests showed that PEEK resin is more notch sensitive than RTM epoxy. Of greater significance, it was found that the 3D is less notch sensitive than the 2D. Unnotched compression tests indicated, as did the tension tests, that the 2D is stronger, stiffer, and has higher elongation at failure than the RTM epoxy. The most encouraging results were from compression after impact. The 3D braided composite showed a compression after impact failure stress equal to 92 percent of the unimpacted specimen. The 2D braided composite failed at about 67 percent of the unimpacted specimen. Higher damage tolerance is observed in textiles over conventional composite materials. This is observed in the results, especially in the 3D braided materials.

Norman, Timothy L.↗
NASA NTRS1990

Compression behavior of graphite-epoxy and graphite-thermoplastic panels with circular holes or impact damage

An experimental investigation of the compression behavior of laminated specimens made from graphite-epoxy tape (AS4-3502), graphite-thermoplastic tape (AS4-PEEK), and graphite-thermoplastic fabric (AS4-PEEK) was conducted. Specimens with five different stacking sequences were loaded to failure in uniaxial compression. Some of the specimens had central circular holes with diameters up to 65 percent of the specimen width. Other specimens were subjected to low speed impact with impact energy up to 30 J prior to compressive loading. This investigation indicates that graphite-thermoplastic specimens with holes have up to 15 percent lower failure stresses and strains than graphite-epoxy specimens with the same stacking sequence and hole size. However, graphite-thermoplastic specimens subjected to low speed impact have up to 15 percent higher failure stresses and strains than graphite-epoxy specimens with the same stacking sequence and impact energy. Compression tests of graphite-thermoplastic specimens constructed of unidirectional tape and of fabric indicate that the material form has little effect on failure strains in specimens with holes or low speed impact damage.

Jegley, Dawn C.↗
NASA NTRS1996

Atomic Oxygen and Space Environment Effects on Aerospace Materials Flown with EOIM-3 Experiment

Polymer materials samples mounted on a passive carrier tray were flown aboard the STS-46 Atlantis shuttle as complement to the EOIM-3 (Evaluation of Oxygen Interaction with Materials) experiment to evaluate the effects of atomic oxygen on the materials and to measure the gaseous shuttle bay environment. The morphological changes of the samples produced by the atomic oxygen fluence of 2.07 x 10(exp 20) atoms/cm(exp 2) are being reported. The changes have been verified using Electron Spectroscopy for Chemical Analysis (ESCA), gravimetric measurement, microscopic observations and thermo-optical measurements. The samples, including Kapton, Delrin, epoxies, Beta Cloth, Chemglaze Z306, silver Teflon, silicone coatings, 3M tape and Uralane and Ultem, PEEK, Victrex (PES), Polyethersulfone and Polymethylpentene thermoplastic, have been characterized by their oxygen reaction efficiency on the basis of their erosion losses and the oxygen fluence. Those efficiencies have been compared to results from other experiments, when available. The efficiencies of the samples are all in the range of E-24 g/atom. The results indicate that the reaction efficiencies of the reported materials can be grouped in about three ranges of values. The least affected materials which have efficiencies varying from 1 to 10(exp 25) g/atom, include silicones, epoxies, Uralane and Teflon. A second group with efficiency from 10 to 45(exp 25) g/atom includes additional silicone coatings, the Chemglaze Z306 paint and Kapton. The third range from 50 to 75(exp 25) includes organic compound such as Pentene, Peek, Ultem, Sulfone and a 3M tape. A Delrin sample had the highest reaction efficiency of 179(exp 25) g/atom. Two samples, the aluminum Beta cloth X389-7 and the epoxy fiberglass G-11 nonflame retardant, showed a slight mass increase.

Scialdone, John J.↗
NASA NTRS2000

A Damage Resistance Comparison Between Candidate Polymer Matrix Composite Feedline Materials

As part of NASAs focused technology programs for future reusable launch vehicles, a task is underway to study the feasibility of using the polymer matrix composite feedlines instead of metal ones on propulsion systems. This is desirable to reduce weight and manufacturing costs. The task consists of comparing several prototype composite feedlines made by various methods. These methods are electron-beam curing, standard hand lay-up and autoclave cure, solvent assisted resin transfer molding, and thermoplastic tape laying. One of the critical technology drivers for composite components is resistance to foreign objects damage. This paper presents results of an experimental study of the damage resistance of the candidate materials that the prototype feedlines are manufactured from. The materials examined all have a 5-harness weave of IM7 as the fiber constituent (except for the thermoplastic, which is unidirectional tape laid up in a bidirectional configuration). The resin tested were 977-6, PR 520, SE-SA-1, RS-E3 (e-beam curable), Cycom 823 and PEEK. The results showed that the 977-6 and PEEK were the most damage resistant in all tested cases.

Nettles, A. T↗