Process for interfacial polymerization of pyromellitic dianhydride and 1,2,4, 5-tetraamino-benzene Patent
Process for interfacial polymerization of pyromellitic dianhydride and tetraamino benzene
Bell, V. L., Jr.↗
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New aromatic silicon-containing polyamides
The experiments described were aimed at studying systematically the effect of silyl linkages on the thermogravimetric and thermomechanical properties of aromatic polyamides. Specifically, 18 aromatic silicon-containing polyamides were synthesized via interfacial polymerization of six silicon-containing diacid chlorides with 3,3-prime-diaminodiphenylmethane, 3,3-prime-diaminobenzophenone, and 1-(3-prime-aminobenzyl)-4-(3-double prime-aminobenzoyl)benzene. All polyamides were soluble in m-cresol and N,N-dimethylacetamide, and had glass transition temperatures between 178 and 254 C. Thermogravimetric analysis conducted in static air on film specimens showed 5 and 10 percent weight losses between 331 and 400 C and 354 and 440 C, respectively. The potential gain in processability engendered by incorporation of silane substituents was offset in most cases by substantial losses in thermo-oxidative stability.
Pratt, J. R.↗
Syntheses and thermal stabilities of polyamides from 2,2'-bithiophene-5,5'-dicarbonyl dichloride and diamines
The properties of 12 polymers derived from 2,2'-bithiophene-5,5'-dicarbonyl dichloride are analyzed. The solution and interfacial polymerizations of 2,2'-bithiophene-5,5'-dicarbonyl dichloride are described. It is observed that due to high glass transition temperatures and the lack of flexibility of the polyamide of 2,2'-bithiophene-5,5'-dicarbonyl dichloride most of the polymers failed to fabricate into fibers or films. The data reveal that the polyamides formed from terphenyl ether form a tough, heat-pressed film; the polyamides made from aromatic diamides show great thermal stability; and the polyamides derived from aliphatic or benzylic diamides display no thermal stability.
Barber, Patrick G.↗
pH Sensitive Microcapsules for Delivery of Corrosion Inhibitors
A considerable number of corrosion problems can be solved by coatings. However, even the best protective coatings can fail by allowing the slow diffusion of oxygen and moisture to the metal surface. Corrosion accelerates when a coating delaminates. Often, the problems start when microscopic nicks or pits on the surface develop during manufacturing or through wear and tear. This problem can be solved by the incorporation of a self-healing function into the coating. Several new concepts are currently under development to incorporate this function into a coating. Conductive polymers, nanoparticles, and microcapsules are used to release corrosion-inhibiting ions at a defect site. The objective of this investigation is to develop a smart coating for the early detection and inhibition of corrosion. The dual function of this new smart coating system is performed by pH-triggered release microcapsules. The microcapsules can be used to deliver healing agents to terminate the corrosion process at its early stage or as corrosion indicators by releasing dyes at the localized corrosion sites. The dyes can be color dyes or fluorescent dyes, with or without pH sensitivity. Microcapsules were formed through the interfacial polymerization process. The average size of the microcapsules can be adjusted from 1 to 100 micron by adjusting the emulsion formula and the microcapsule forming conditions. A typical microcapsule size is around 10 microns with a narrow size distribution. The pH sensitivity of the microcapsule can also be controlled by adjusting the emulsion formula and the polymerization reaction time. Both corrosion indicator (pH indicator) and corrosion inhibitor containing microcapsules were formed and incorporated into paint systems. Test panels of selected steels and aluminum alloys were painted using these paints. Testing of compatibility between the microcapsule system and different paint systems are in progress. Initial experiments with the microcapsule containing paint show visible color changes at induced corrosion sites and improvement of corrosion protection. Further investigation of the performance of the coating using electrochemical techniques and long term exposure are currently underway.
Li, Wenyan↗
Effect of Interfacial characteristics of metal clad polymeric substrates on electrical high frequency interconnection performance
Etched metallic conductor lines on metal clad polymeric substrates are used for electronic component interconnections. Significant signal losses are observed for microstrip conductor lines used for interconnecting high frequency devices. At these frequencies, the electronic signal travels closer to the metal-polymer interface due to the skin effect. Copper-teflon interfaces were characterized by scanning electron microscopy (SEM) and Auger electron spectroscopy (AES) to determine the interfacial properties. Data relating roughness of the copper film to signal losses was compared to theory. Films used to enhance adhesion are found, to contribute to these losses.
Bhasin, K. B.↗
Study of changes in properties of solar sail materials from radiation exposure
Techniques for monitoring changes in preparation of solar sail materials resulting from space radiation simulation, stressing (e.g., thermal, mechanical) and exposure to terrestrial environments are developed. The properties of interest are: metallic coating deterioration, polymeric film deterioration, interfacial debonding and possible metallic coating diffusion into the polymeric film. Four accelerated tests were devised to simulate the possible degradation processes mentioned above. These four tests are: a thermal shock test to simulate the wide variation of temperature expected in space (260 C to -100 C), a cyclic temperature test to stimulate the 6 minute temperature cycle anticipated in space, a mechanical vibration test to simulate mechanical bonding, folding and handling, and a humidity test to simulate terrestrial environment effects. The techniques for monitoring property changes are: visual and microscopic examination, ellipsometry, surface potential difference (SPD), photoelectron emission (PEE), and water contact angles.
Smith, T.↗
Molecular correlations with fracture in fibers and granular-filled composites
Results are presented for an experimental electron spin resonance study of chain-scission kinetics in oriented nylon fibers and in granular-filled elastomer composites. A reaction-rate molecular model is proposed as a tool to predict failure under various loadings. The model assumes a statistical distribution in stress on the polymeric chain structure. Interfacial failure in the filled composites is examined. Failure at the interface between the filler and the matrix may be largely adhesive or cohesive, depending on the magnitude of the interactive forces. It appears that the mechanical behavior of both single-component and filled composites depends on the composite nature of the structure. The electron spin resonance technique is shown to be suitable for experimental observation of phenomena directly related to atomic occurrences.
Devries, K. L.↗
Chemical Modification of the Surface of High Modulus Carbon Fibers
The deposition of selected monomers on the surface of high modulus carbon fibers was studied. The fundamental principles which provide the basis for the design of a predictable interfacial bond between carbon fibers and polymeric matrices are described.
Source record↗
Molecular Probe Fluorescence Monitoring of Polymerization
This project investigated the feasibility of using fluorescence spectroscopy to determine viscosity of polymer/monomer in support of Transient Interfacial Phenomena in Miscible Polymer Systems (TIPMPS). This project will attempt to measure gradient induced flow at a miscible interface during and / or after in-flight polymerization of dodecyl acrylate (lauryl acrylate). Concentration and temperature gradients will be intentionally introduced during polymerization and the resultant fluid flow determined by Particle Imaging Velocimetry (PIV). This report describes an investigation of the feasibility of using fluorescence of a probe molecule to monitor viscosity and/or concentration during and after polymerization. The probe used was pyrene which has been shown to be sensitive to its local environment in methyl methacrylate.
Patrick Bunton↗
Characterization of Polyimide Foams for Ultra-Lightweight Space Structures
Ultra-lightweight materials have played a significant role in nearly every area of human activity ranging from magnetic tapes and artificial organs to atmospheric balloons and space inflatables. The application range of ultra-lightweight materials in past decades has expanded dramatically due to their unsurpassed efficiency in terms of low weight and high compliance properties. A new generation of ultra-lightweight materials involving advanced polymeric materials, such as TEEK (TM) polyimide foams, is beginning to emerge to produce novel performance from ultra-lightweight systems for space applications. As a result, they require that special conditions be fulfilled to ensure adequate structural performance, shape retention, and thermal stability. It is therefore important and essential to develop methodologies for predicting the complex properties of ultra-lightweight foams. To support NASA programs such as the Reusable Launch Vehicle (RLV), Clark Atlanta University, along with SORDAL, Inc., has initiated projects for commercial process development of polyimide foams for the proposed cryogenic tank integrated structure (see figure 1). Fabrication and characterization of high temperature, advanced aerospace-grade polyimide foams and filled foam sandwich composites for specified lifetimes in NASA space applications, as well as quantifying the lifetime of components, are immensely attractive goals. In order to improve the development, durability, safety, and life cycle performance of ultra-lightweight polymeric foams, test methods for the properties are constant concerns in terms of timeliness, reliability, and cost. A major challenge is to identify the mechanisms of failures (i.e., core failure, interfacial debonding, and crack development) that are reflected in the measured properties. The long-term goal of the this research is to develop the tools and capabilities necessary to successfully engineer ultra-lightweight polymeric foams. The desire is to reduce density at the material and structural levels, while at the same time maintaining or increasing mechanical and other properties.
Meador, Michael↗
Secondary Li battery incorporating 12-Crown-4 ether
A rechargeable lithium battery which utilizes a polyethylene oxide (PEO) solid polymeric electrolyte complexed with a lithium salt is disclosed. The conductivity is increased an order of magnitude and interfacial charge transfer resistance is substantially decreased by incorporating a minor amount of 12-Crown-4 ether in the PEO-lithium salt solid electrolyte film. Batteries containing the improved electrolyte permit operation at a lower temperature with improved efficiency.
Nagasubramanian, Ganesan↗
Characterization of surfaces
Low gravity biotechnology experiments indicate a need to better understand and control a host of liquid-solid interfacial phenomena which reduce the efficiency of bioseparations methods on earth as well as in space. We have improved and utilized polymeric and silane derivatives, developed in association with MSFC, in order to control such phenomena. The objectives of the proposed research have been obtained. They were to improve NASA-patented coatings capable of controlling macromolecular adsorption, electroosmosis, and particle electrophoresis over a wide range of pH, and to further characterize the ability of polymeric coatings to control wall wetting interactions. To date this research has resulted in six publications and four abstracts. It has also aided researchers at MSFC with studies on the electrophoresis of large DNA molecules in free solution. It will continue to enhance NASA's efforts to exploit the space environment to enhance knowledge of phenomena relevant to biotechnology, and obtain bioseparations currently unobtainable on Earth. Abstracts from the 1994 ACS Meeting in Birmingham are attached.
Vanalstine, James M.↗
Modeling Geometry and Progressive Failure of Material Interfaces in Plain Weave Composites
A procedure combining a geometrically nonlinear, explicit-dynamics contact analysis, computer aided design techniques, and elasticity-based mesh adjustment is proposed to efficiently generate realistic finite element models for meso-mechanical analysis of progressive failure in textile composites. In the procedure, the geometry of fiber tows is obtained by imposing a fictitious expansion on the tows. Meshes resulting from the procedure are conformal with the computed tow-tow and tow-matrix interfaces but are incongruent at the interfaces. The mesh interfaces are treated as cohesive contact surfaces not only to resolve the incongruence but also to simulate progressive failure. The method is employed to simulate debonding at the material interfaces in a ceramic-matrix plain weave composite with matrix porosity and in a polymeric matrix plain weave composite without matrix porosity, both subject to uniaxial cyclic loading. The numerical results indicate progression of the interfacial damage during every loading and reverse loading event in a constant strain amplitude cyclic process. However, the composites show different patterns of damage advancement.
Hsu, Su-Yuen↗
Leakage-current properties of encapsulants
A theoretical modeling of leakage current in ethylene vinyl acetate (EVA) and polyvinyl butyral (PVB) modules is being developed and is described. The modeling effort derives mathematical relationships for the bulk and surface conductivites of EVA and PVB, the surface conductivities of glass and polymeric films, and the EVA and PVB pottants, all as functions of environmental parameters. Results from the modeling indicate that for glass/EVA, the glass surface controls the interfacial conductivity, although EVA bulk conductivity controls total leakage current. For PVB/glass, the interface conductivity controls leakage currents for relative humidity (RH) less than 40 to 50%, but PVB bulk conductivity controls leakage current above 50% RH.
Wen, L. C.↗
Modeling of delamination damage evolution in laminated composites subjected to low velocity impact
This study examines the delamination evolution, under quasi-static conditions, of laminated polymeric composites with mechanically nonlinear resin rich interfaces. The constitutive behavior of the interface is represented by two models developed by Needleman and Tvegaard. These models assumed that the interfacial tractions, a function of only the interfacial displacement, will behave similarly to the interatomic forces generated during the interatomic seperation. The interface material's parameters control the load at which the delamination growth initiates and the final delamination size. A wide range of damage accumulation responses have been obtained by varying the model parameters. These results show that Tvergaard's model has been found to be better suited of the two models in predicting damage evolution for the configurations examined.
Lo, David C.↗
Frontal Polymerization in Microgravity Summary of Research
The project began with frontal polymerization (FP). We studied many aspects of FP on the ground and performed two successful weeks of flying on the KC-135. The project evolved into the current flight investigation, Transient Interfacial Phenomena in Miscible Polymer Systems (TIPMPS), as we recognized that an essential question could best be studied using a non-frontal approach. We present detailed results from our ground-based work on FP, KC-135 results and the background, justification and numerical work for the TIPMPS project.
Pojman, John A.↗
Improving Tracer Particle Surface Properties for Wind Tunnel Research
The surface properties of micron size polystyrene latex microspheres (PSLs) modified with quaternary alkylammonium (QA) surfactants were investigated, with a focus on the relationship between surface chemistry and adhesion. These investigations were motivated by the need to develop non-fouling tracer particles for wind tunnel studies. The goals were to relate the work of adhesion between particles and substrates to the type and amount of QA modifier in order to optimize the performance of PSL tracers. Surfactant-free emulsion polymerization (SFEP) can produce PSLs for wind tunnel tracers. Covalentlybound charged groups (derived from the initiator) stabilize PSL surfaces in water. This work used PSLs with anionic surface groups. Previous studies indicated that surface-bound charged groups on PSLs have a significant impact on their interfacial energy. Modifying charged surface groups therefore offers a method to modulate PSL interfacial properties. In this work, PSLs and films were modified by adsorption of QA surfactants.
Schmitz, Russell C.↗
Modeling Initial Stage of Ablation Material Pyrolysis: Graphitic Precursor Formation and Interfacial Effects
Reactive molecular dynamics simulations are used to study initial stage of pyrolysis of ablation materials and their composites with carbon nanotubes and carbon fibers. The products formed during pyrolysis are characterized and water is found as the primary product in all cases. The water formation mechanisms are analyzed and the value of the activation energy for water formation is estimated. A detailed study on graphitic precursor formation reveals the presence of two temperature zones. In the lower temperature zone (less than 2000 K) polymerization occurs resulting in formation of large, stable graphitic precursors, and in the high temperature zone (greater than 2000 K) polymer scission results in formation of short polymer chains/molecules. Simulations performed in the high temperature zone on the phenolic resin composites (with carbon nanotubes and carbon fibers) shows that the presence of interfaces had no substantial effect on the chain scission rate or the activation energy value for water formation.
Desai, Tapan G.↗