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At least 145 records · Page 8

Microscopy and microstructure of Shuttle thermal protection system materials

Examples of the contribution of microstructural analysis to the development of the Space Shuttle tile insulation system are presented, with photographic examples of the scanning electron microscope (SEM) investigations. After the basic thermal protection system materials had been selected, it was neccessary to analyze the mechanical responses of the combined materials; which included: (1) the polymer strain isolation pad (SIP), (2) the room temperature-vulcanizing silicone rubber bond, (RTV), and (3) rigid ceramic fiber reusable surface insulation (RSI). Microstructural analysis was used to provide information on deformation and fracture mechanisms, load transfer mechanisms, and structural alterations occurring before final failure. Both quantitative and qualitative information was obtained in the open, three-dimensional fibrous structures of the ceramic tiles by means of novel techniques of encapsulation and dissolution.

Newquist, C. W.↗

Kink band formation in unidirectional composites under compression

The kink band formation in unidirectional composites under compression was studied with the help of optical and scanning electron microscopy. Materials studied included graphite/epoxy, S-2 glass/epoxy, and Kevlar 49/epoxy composites. The kink bands in the graphite/epoxy and glass/epoxy composites were initiated by fiber microbuckling while those in the Kevlar/epoxy composite were triggered by microkinking in the fibers themselves. Fracture surfaces of the graphite/epoxy composites showed fibers broken in bending and fiber segments tilted in the direction of slip. The kink band formation depended not only on the constituent material properties but also on the kinematic constraints imposed. Both primary and secondary kink bands were observed in the graphite/epoxy specimens, but only primary kink bands were present in the other two composites because of higher lateral flexibility of the specimen during testing.

Sohi, M. M.↗

Real-Time Keratometer

Optical/electronic keratometer system produces contour map of corneal surface illuminated by infrared light pulses. Prevents operator error and eliminates need to apply fluorescent liquids to cornea. Keratometer provides both video display and numerical recording for corneal-transplant and radial-keratotomy surgery and for contact-lens fitting. Optical system of keratometer, circular grating pattern transmitted to corneal surface reflected onto identical circular grating on surface of fiber plate, producing Moire pattern. Data-analysis-and-display mode, laser light pulsed, and Moire pattern converted to digital information in frame grabber. Digital picture information sent to computer for processing and display.

Frazer, Robert E.↗

Treating Fibrous Insulation to Reduce Thermal Conductivity

A chemical treatment reduces the convective and radiative contributions to the effective thermal conductivity of porous fibrous thermal-insulation tile. The net effect of the treatment is to coat the surfaces of fibers with a mixture of transition-metal oxides (TMOs) without filling the pores. The TMO coats reduce the cross-sectional areas available for convection while absorbing and scattering thermal radiation in the pores, thereby rendering the tile largely opaque to thermal radiation. The treatment involves a sol-gel process: A solution containing a mixture of transition-metal-oxide-precursor salts plus a gelling agent (e.g., tetraethylorthosilicate) is partially cured, then, before it visibly gels, is used to impregnate the tile. The solution in the tile is gelled, then dried, and then the tile is fired to convert the precursor salts to the desired mixed TMO phases. The amounts of the various TMOs ultimately incorporated into the tile can be tailored via the concentrations of salts in the solution, and the impregnation depth can be tailored via the viscosity of the solution and/or the volume of the solution relative to that of the tile. The amounts of the TMOs determine the absorption and scattering spectra.

Zinn, Alfred↗

Characterization of low thermal conductivity PAN-based carbon fibers

The microstructure and surface chemistry of eight low thermal conductivity (LTC) PAN-based carbon fibers were determined and compared with PAN-based fibers heat treated to higher temperatures. Based on wide-angle x ray diffraction, the LTC PAN fibers all appear to have a similar turbostratic structure with large 002 d-spacings, small crystallite sizes, and moderate preferred orientation. Limited small-angle x ray scattering (SAXS) results indicate that, with the exception of LTC fibers made by BASF, the LTC fibers do not have well developed pores. Transmission electron microscopy shows that the texture of the two LTC PAN-based fibers studied (Amoco T350/23X and /25X) consists of multiple sets of parallel, wavy, bent layers that interweave with each other forming a complex three dimensional network oriented randomly around the fiber axis. X ray photoelectron spectroscopy (XPS) analysis finds correlations between heat treated temperatures and the surface composition chemistry of the carbon fiber samples.

Katzman, Howard A.↗

Coating Carbon Fibers With Platinum

A process for coating carbon fibers with platinum has been developed. The process may also be adaptable to coating carbon fibers with other noble and refractory metals, including rhenium and iridium. The coated carbon fibers would be used as ingredients of matrix/fiber composite materials that would resist oxidation at high temperatures. The metal coats would contribute to oxidation resistance by keeping atmospheric oxygen away from fibers when cracks form in the matrices. Other processes that have been used to coat carbon fibers with metals have significant disadvantages: Metal-vapor deposition processes yield coats that are nonuniform along both the lengths and the circumferences of the fibers. The electrical resistivities of carbon fibers are too high to be compatible with electrolytic processes. Metal/organic vapor deposition entails the use of expensive starting materials, it may be necessary to use a furnace, and the starting materials and/or materials generated in the process may be hazardous. The present process does not have these disadvantages. It yields uniform, nonporous coats and is relatively inexpensive. The process can be summarized as one of pretreatment followed by electroless deposition. The process consists of the following steps: The surfaces of the fiber are activated by deposition of palladium crystallites from a solution. The surface-activated fibers are immersed in a solution that contains platinum. A reducing agent is used to supply electrons to effect a chemical reduction in situ. The chemical reduction displaces the platinum from the solution. The displaced platinum becomes deposited on the fibers. Each platinum atom that has been deposited acts as a catalytic site for the deposition of another platinum atom. Hence, the deposition process can also be characterized as autocatalytic. The thickness of the deposited metal can be tailored via the duration of immersion and the chemical activity of the solution.

Effinger, Michael R.↗

Silica Reusable Surface Insulation Improvement Research

Fiber characterization, fabrication processes, physical properties, and thermal responses are investigated to improve silica reusable surface insulation tiles. Criteria for fiber selection on the basis of chemical composition, shrinkage, and devitrification have been defined and a simple process for fabricating silica surface insulation materials has been developed that produces only 5% shrinkage and no devitrification of tiles at 1533 K in ten hours. Anisotropic tile with improved weak direction strength has been fabricated using conventional molding techniques.

Goldstein, H. E.↗

Feasibility and process scale-up low cost alumina fibers for advanced Re-usable Surface Insulation (RSI)

The objective of this program was to establish feasibility of a process to produce low cost aluminum oxide fibers having sufficient strength, flexibility, and thermal stability for multiple re-use at temperatures to 1480 C in advanced RSI type heat shields for reentry vehicles. Using bench-scale processing apparatus, the Alcoa 'Saphiber' process was successfully modified to produce nominally 8 microns diameter polycrystalline alpha-alumina fiber. Thermal stability was demonstrated in vacuum reheating tests to 1371 C and in atmospheric reheating to 1483 C. Individual fiber properties of strength, modulus, and flexibility were not determined because of friability and short length of the fiber. Rigidized tile produced from fiber of nominally 8, 20 and 40 micron diameter had thermal conductivities significantly higher than those of RSI SiO2 or mullite at relatively low temperature but became comparable above about 1000 C. Tile densities were high due to short fiber length, especially in the coarser diameter fiber. No significant effect of fiber diameter on thermal properties could be determined form the data. Mechanical properties of tiles deteriorated as fiber diameter increased.

Pearson, A.↗

Thermomechanical Characterization of SiC Fiber Tows and Implications for CMC

In order to better understand SiC fiber behavior within CMC microstructures, mechanical tests were performed on multifilament tows consisting of different types of as produced and pretreated fibers. Tensile strengths of tows and single fibers were measured at room temperature for nonstoichiometric Hi-Nicalon and ZMI fibers and for stoichiometric Hi-Nicalon-S, Tyranno SA. and Sylramic fibers. Based on simple bundle theory, measured strengths for as-produced and sized tows were in general agreement with the single fiber results. However, after sizing removal under inert conditions, tow strengths for the coarser grained stoichiometric fibers were typically lower than those predicted from individual fiber data. This effect is attributed to enhanced fiber-fiber mechanical interaction caused by sizing removal from the rough surfaces of these fibers. In support of this, tow strengths remained high for those fiber types with fine grains or excess surface carbon; and, when re-coated with a BN interphase coating, tow strengths for the coarser grained fibers returned to their as-produced values. When the tows were pretreated in air at intermediate temperatures, tow strengths decreased in a manner that could be correlated with the oxidation characteristics of each fiber type as measured by thermogravimetric analysis. The creep and rupture properties of Hi-Nicalon and Sylramic tows were also measured in air and argon from 1200 to 1400 C. Although displaying transient and environmental effects similar to single fibers, the tows crept faster at short times and slower at long times. This resulted in the tow rupture strengths at long time being much greater than the rupture strengths of single fibers. The CMC implications of the tow results are discussed, as well as the benefits and limitations of tow testing.

Yun, H. M.↗

Polymeric electrolytic hygrometer

An improved flow-through electrolytic hygrometer is described which utilizes a long lasting oxidation-resistant, hollow fiber formed from persulfonic acid substituted polytetrafluoroethylene having closely spaced noble metal electrodes in contact with the inner and outer surfaces of the fiber. The fiber is disposed within a chamber so that the moisture-bearing gas passes in contact with at least one surface of the fiber. The electrodes are connected in series to a dc voltage supply and an ammeter. As the gas passes through the chamber, moisture absorbed into the wall of the fiber is electrolyzed to hydrogen and oxygen by the closely spaced electrodes. The amount of electricity required for electrolysis is proportional to the absorbed moisture and is observed on the ammeter.

Lawson, D. D.↗

Electrospun Nanofiber Coating of Fiber Materials: A Composite Toughening Approach

Textile-based composites could significantly benefit from local toughening using nanofiber coatings. Nanofibers, thermoplastic or otherwise, can be applied to the surface of the fiber tow bundle, achieving toughening of the fiber tow contact surfaces, resulting in tougher and more damage-resistant/tolerant composite structures. The same technique could also be applied to other technologies such as tape laying, fiber placement, or filament winding operations. Other modifications to the composite properties such as thermal and electrical conductivity could be made through selection of appropriate nanofiber material. Control of the needle electric potential, precursor solution, ambient temperature, ambient humidity, airflow, etc., are used to vary the diameter and nanofiber coating morphology as needed. This method produces a product with a toughening agent applied to the fiber tow or other continuous composite precursor material where it is needed (at interfaces and boundaries) without interfering with other composite processing characteristics.

Kohlman, Lee W.↗

High surface area, low weight composite nickel fiber electrodes

The energy density and power density of light weight aerospace batteries utilizing the nickel oxide electrode are often limited by the microstructures of both the collector and the resulting active deposit in/on the collector. Heretofore, these two microstructures were intimately linked to one another by the materials used to prepare the collector grid as well as the methods and conditions used to deposit the active material. Significant weight and performance advantages were demonstrated by Britton and Reid at NASA-LeRC using FIBREX nickel mats of ca. 28-32 microns diameter. Work in our laboratory investigated the potential performance advantages offered by nickel fiber composite electrodes containing a mixture of fibers as small as 2 microns diameter (Available from Memtec America Corporation). These electrode collectors possess in excess of an order of magnitude more surface area per gram of collector than FIBREX nickel. The increase in surface area of the collector roughly translates into an order of magnitude thinner layer of active material. Performance data and advantages of these thin layer structures are presented. Attributes and limitations of their electrode microstructure to independently control void volume, pore structure of the Ni(OH)2 deposition, and resulting electrical properties are discussed.

Johnson, Bradley A.↗

Improvement of Reusable Surface Insulation (RSI) materials

The mullite fiber based hardened compacted fibers (HCF) type of reusable surface insulation was further developed for use in the Space Shuttle Program. Two hundred fifty formulations of fiber mixtures, fillers, binders, and organic processing aids were made using mullite fibers as the basic ingredient. Most of the work was accomplished on 15-lb/cu ft material. It was established that higher density materials are stronger with strength values as high as 250 lb/sq in. in tension. New measurement techniques and equipment were developed for accurate determination of strength and strain to failure. Room temperature to 2300 F stress-strain relationships were made. The room temperature tensile modulus of elasticity is 61,700 lb/sq in. and the strain at failure is 0.165 percent, typically, when measured longitudinally parallel to the long axes of the fibers. Thermal insulating effectiveness was increased 20 percent by reducing the diameter of some of the fibers in the material. Improvements were made in density uniformity and strength uniformity in a block of HCF by mixing improvements and by the use of organic additives. Specifications were established on the materials and processes used in making the insulation.

Blome, J. C.↗

Surface and interfacial properties of carbon fibers

Differences in the adhesion of three carbon fibers (Hercules AS1 and AS4, and Hysol-Grafil XAS) to polycarbonate (PC) have been shown to correlate with the absorptivity of PC on the three fiber types. The absorptivity (energy of absorption) was determined using retention time liquid chromatography and the adhesion was measured using the single embedded filament tensile test. A correlation was also found between adhesion strength and the O/N surface element ratio using XPS analysis. The chemical details for these correlations have not yet been determined. A study of filament fracture statistics has been initiated using single and multiple embedded filament tensile tests. Filament fracture has been measured as a function of strain and for different interfiber distances. Preliminary results indicate that fiber fracture is a discontinuous function of increasing strain and may in fact occur at discrete strain intervals. Fiber-fiber interaction effects on fiber fracture have been found for interfiber distances of up to two to three fiber diameters.

Bascom, W. D.↗

A micrographic study of bending failure in five thermoplastic/carbon fiber composite laminates

The local deformation and failure sequences of five thermoplastic matrix composites were microscopically observed while bending the samples in a small fixture attached to a microscope stage. The themoplastics are polycarbonate, polysulfone, polyphenylsulfide, polyethersulfone, and polyetheretherketone. Comparison was made to an epoxy matrix composite, 5208/T-300. Laminates tested are (0/90) sub 2S, with outer ply fibers parallel to the beam axis. Four point bending was used at a typical span-to-thickness ratio of 39:1. It was found that all of the thermoplastic composites failed by abrupt longitudinal compression buckling of the outer ply. Very little precursory damage was observed. Micrographs reveal typical fiber kinking associated with longitudinal compression failure. Curved fracture surfaces on the fibers suggest they failed in bending rather than direct compression. Delamination was suppressed in the thermoplastic composites, and the delamination that did occur was found to be the result of compression buckling, rather than visa-versa. Microbuckling also caused other subsequent damage such as ply splitting, transverse ply shear failure, fiber tensile failure, and transverse ply cracking.

Yurgartis, S. W.↗

A micrographic study of bending failure in five thermoplastic-carbon fibre composite laminates

The local deformation and failure sequences of five thermoplastic matrix composites were microscopically observed while bending the samples in a small fixture attached to a microscope stage. The thermoplastics are polycarbonate, polysulfane, polyphenylsulfide, polyethersulfane, and polyetheretherketone. Comparison was made to an epoxy matrix composite, 5208/T-300. Laminates tested are (0/90) sub 2S, with outer ply fibers parallel to the beam axis. Four point bending was used at a typical span-to-thickness ratio of 39:1. It was found that all of the thermoplastic composites failed by abrupt longitudinal compression buckling of the outer ply. Very little precursory damage was observed. Micrographs reveal typical fiber kinking associated with longitudinal compression failure. Curved fracture surfaces on the fibers suggest they failed in bending rather than direct compression. Delamination was suppressed in the thermoplastic composites, and the delamination that did occur was found to be the result of compression buckling, rather than vice-versa. Microbuckling also caused other subsequent damage such as ply splitting, transverse ply shear failure, fiber tensile failure, and transverse ply cracking.

Yurgartis, S. W.↗

Intermediate Temperature Stress Rupture of a Woven Hi-Nicalon, BN-Interphase, SiC Matric Composite in Air

Woven Hi-Nicalon (TM) reinforced melt-infiltrated SiC matrix composites were tested under tensile stress-rupture conditions in air at intermediate temperatures. A comprehensive examination of the damage state and the fiber properties at failure was performed. Modal acoustic emission analysis was used to monitor damage during the experiment. Extensive microscopy of the composite fracture surfaces and the individual fiber fracture surfaces was used to determine the mechanisms leading to ultimate failure. The rupture properties of these composites were significantly worse than expected compared to the fiber properties under similar conditions. This was due to the oxidation of the BN interphase. Oxidation occurred through the matrix cracks that intersected the surface or edge of a tensile bar. These oxidation reactions resulted in minor degradation to fiber strength and strong bonding of the fibers to one another at regions of near fiber-to-fiber contact. It was found that two regimes for rupture exist for this material: a high stress regime where rupture occurs at a fast rate and a low stress regime where rupture occurs at a slower rate. For the high stress regime, the matrix damage state consisted of through thickness cracks. The average fracture strength of fibers that were pulled-out (the final fibers to break before ultimate failure) was controlled by the slow-crack growth rupture criterion in the literature for individual Hi-Nicalon (TM) fibers. For the low stress regime, the matrix damage state consisted of microcracks which grew during the rupture test. The average fracture strength of fibers that were pulled-out in this regime was the same as the average fracture strength of individual fibers pulled out in as-produced composites tested at room temperature.

Morscher, Gregory N.↗