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NASA NTRS2002

Phenylethynyl Containing Reactive Additives

Phenylethynyl containing reactive additives were prepared from aromatic diamines containing phenylethynyl groups and various ratios of phthalic anhydride and 4-phenylethynylphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pyrrolidinone to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.

John W Connell↗

NASA NTRS2002

Assembly of Colloidal Materials Using Bioadhesive Interactions

We have pursued the use of biological crosslinking molecules of several types to make colloidal materials at relatively low volume fraction of colloidal particles. The objective is to make binary alloys of colloidal particles, made of two different colloidal particles coated with complementary biological lock-and-key binding molecules, which assemble due to the biological specificity. The long-term goal is to use low affinity lock-and-key biological interactions, so that the can anneal to form crystalline states. We have used a variety of different surface chemistries in order to make colloidal materials. Our first system involved using selectin-carbohydrate (sialyl-Lewis) interactions; this chemistry is derived from immune system. This chemical interaction is of relatively low affinity, with timescales for dissociation of several seconds. Furthermore, the adhesion mediated by these molecules can be reversed by the chelation of calcium atoms; thus assembled structures can be disassembled reversibly. Our second system employed avidin-biotin chemistry. This well-studied system is of high affinity, and is generally irreversible on a laboratory time-scale. Thus, we would expect selectin-carbohydrate interactions at high molecular density and avidin-biotin interactions to give kinetically-trapped structures; however, at low densities, we would expect significant differences in the structure and dynamics of the two materials, owing to their very different release rates. We have also begun to use a third chemistry - DNA hybridization. By attaching single stranded DNA oligonucleotide chains to beads, we can drive the assembly of colloidal materials by hybridization of complementary DNA chains. It is well known that DNA adenosine-thymine (A-T) and guanine-cytosine (G-C) bases hybridize pairwise with a Gibbs free energy change of 1.7 kcal/mol per base; thus, the energy of the assembly can be modulated by altering the number of complementary bases in the DNA chains. Using these different crosslinking molecules, we have assembled colloidal materials from different-sized colloidal particles, A and B. In the first sets of experiment, we used high densities of adhesion molecules, and 0.96 micron (A) and 5.5 micron (B) diameter particles. The high density of adhesion molecules means that the structures are kinetically trapped in nonequilibrium configurations. The structure of the suspension can be varied by changing the number ratio of the two types of colloidal particles, NA and NB, where A is the smaller particle. With carbohydrate-selectin or avidin-biotin interactions, large NA/NB leads to the formation of colloidal micelles, with the large center B particle surrounded by many smaller A particles. As the ratio NA/NB decreases, the structures become more extended, approaching the formation of macro-Rouse polymers - extended linear chains where A beads are connected with intervening small B linkers.

Hammer, Daniel A.↗

NASA NTRS2002

Phenylethynyl Containing Reactive Additives

Phenylethynyl containing reactive additives were prepared from aromatic diamine, containing phenylethvnvl groups and various ratios of phthalic anhydride and 4-phenylethynviphthalic anhydride in glacial acetic acid to form the imide in one step or in N-methyl-2-pvrrolidinone to form the amide acid intermediate. The reactive additives were mixed in various amounts (10% to 90%) with oligomers containing either terminal or pendent phenylethynyl groups (or both) to reduce the melt viscosity and thereby enhance processability. Upon thermal cure, the additives react and become chemically incorporated into the matrix and effect an increase in crosslink density relative to that of the host resin. This resultant increase in crosslink density has advantageous consequences on the cured resin properties such as higher glass transition temperature and higher modulus as compared to that of the host resin.

Connell, John W.↗

NASA NTRS2002

Relative Navigation of Formation-Flying Satellites

This paper compares autonomous relative navigation performance for formations in eccentric, medium and high-altitude Earth orbits using Global Positioning System (GPS) Standard Positioning Service (SPS), crosslink, and celestial object measurements. For close formations, the relative navigation accuracy is highly dependent on the magnitude of the uncorrelated measurement errors. A relative navigation position accuracy of better than 10 centimeters root-mean-square (RMS) can be achieved for medium-altitude formations that can continuously track at least one GPS signal. A relative navigation position accuracy of better than 15 meters RMS can be achieved for high-altitude formations that have sparse tracking of the GPS signals. The addition of crosslink measurements can significantly improve relative navigation accuracy for formations that use sparse GPS tracking or celestial object measurements for absolute navigation.

Long, Anne↗

NASA NTRS2003

Reevaluation of Tetrahydrophthalic Anhydride as an End Cap for Improved Oxidation Resistance in Addition Polyimides

Several substituted 1,2,3,6-tetrahydrophthalic anhydride end caps - including the 3-phenyl, 3-methoxy, 3-trimethylsilyloxy, and 3,6-diphenyl analogs - were synthesized via the Diels-Alder condensation of the corresponding butadienes and maleic anhydride. These anhydrides, as well as the commercially available 3-hydro and 4-methyl analogs, were each ground together with methylenedianiline in a 2:1 ratio and heated gradually from 204 C to 371 C, with the thermolysis followed by NMR. Generally speaking, a transformation via monoimide to bisimide was observed in the lower temperature range, followed by competition between crosslinking and aromatization. We believe that this competition produces a substantial percentage of aromatic product, with the concomitant lowering of the relative amount of crosslinking and is responsible for improving both thermal oxidative stability of tetrahydrophthalic end capped polyimides and their substantial frangibility. The thermolysis of the tetrahydrophthalimides under inert atmosphere dramatically lowers the amount of aromatization hence, the mechanism for aromatization is an oxidative one.

Meador, Mary Ann B.↗

NASA NTRS2003

Relative Navigation Algorithms for Phase 1 of the MMS Formation

This paper evaluates several navigation approaches for the first phase of the Magnetospheric Multiscale (MMS) mission, which consists of a tetrahedral formation of four satellites in highly eccentric Earth orbits of approximately 1.2 by 12 Earth radii at an inclination of 10 degrees. The inter-satellite separation is approximately 10 kilometers near apogees. Navigation approaches were studied using ground station m g e =d two-way Doppler measurements, Global Positioning System (GPS) pseudorange measurements, crosslink range measurements among the members flying in formation, and various combinations of these measurement types. An absolute position accuracy of 10 kilometers or better can be achieved with most of the approaches studied and a relative position accuracy of 100 meters or better can be achieved at apogee in some cases. Among the various approaches studied, the approaches that use a combination of GPS and crosslink measurements were found to be more reliable in terms of absolute and relative navigation accuracies and operational flexibility.

Kelbel, David↗

NASA NTRS2000

How Molecular Structure Affects Mechanical Properties of an Advanced Polymer

density was performed over a range of temperatures below the glass transition temperature. The physical characterization, elastic properties and notched tensile strength all as a function of molecular weight and test temperature were determined. For the uncrosslinked SI material, it was shown that notched tensile strength is a strong function of both temperature and molecular weight, whereas stiffness is only a strong function of temperature. For the crosslinked PETI-SI material, it was shown that the effect of crosslinking significantly enhances the mechanical performance of the low molecular weight material; comparable to that exhibited by the high molecular weight material.

Nicholson, Lee M.↗

NASA NTRS1990

The role of wall calcium in the extension of cell walls of soybean hypocotyls

Calcium crosslinks are load-bearing bonds in soybean (Glycine max (L.) Merr.) hypocotyl cell walls, but they are not the same load-bearing bonds that are broken during acid-mediated cell elongation. This conclusion is reached by studying the relationship between wall calcium, pH and the facilitated creep of frozen-thawed soybean hypocotyl sections. Supporting data include the following observations: 1) 2-[(2-bis-[carboxymethyl]amino-5-methylphenoxy)methyl]-6-methoxy-8-bis[car boxymethyl]aminoquinoline (Quin 2) and ethylene glycol-bis(2-aminoethyl ether)-N,N,N',N'-tetraacetic acid (EGTA) caused only limited facilitated creep as compared with acid, despite removal of comparable or larger amounts of wall calcium; 2) the pH-response curves for calcium removal and acid-facilitated creep were different; 3) reversible acid-extension occurred even after removal of almost all wall calcium with Quin 2; and 4) growth of abraded sections did not involve a proportional loss of wall calcium. Removal of wall calcium, however, increased the capacity of the walls to undergo acid-facilitated creep. These data indicate that breakage of calcium crosslinks is not a major mechanism of cell-wall loosening in soybean hypocotyl tissues.

Non-NASA Center↗

NASA NTRS2001

The gating mechanism of the large mechanosensitive channel MscL

The mechanosensitive channel of large conductance, MscL, is a ubiquitous membrane-embedded valve involved in turgor regulation in bacteria. The crystal structure of MscL from Mycobacterium tuberculosis provides a starting point for analysing molecular mechanisms of tension-dependent channel gating. Here we develop structural models in which a cytoplasmic gate is formed by a bundle of five amino-terminal helices (S1), previously unresolved in the crystal structure. When membrane tension is applied, the transmembrane barrel expands and pulls the gate apart through the S1-M1 linker. We tested these models by substituting cysteines for residues predicted to be near each other only in either the closed or open conformation. Our results demonstrate that S1 segments form the bundle when the channel is closed, and crosslinking between S1 segments prevents opening. S1 segments interact with M2 when the channel is open, and crosslinking of S1 to M2 impedes channel closing. Gating is affected by the length of the S1-M1 linker in a manner consistent with the model, revealing critical spatial relationships between the domains that transmit force from the lipid bilayer to the channel gate.

Non-NASA Center↗

NASA NTRS1996

The effect of nonablative laser energy on joint capsular properties. An in vitro histologic and biochemical study using a rabbit model

The purpose of this study was to evaluate the effect of laser energy at nonablative levels on joint capsular histologic and biochemical properties in an in vitro rabbit model. The medial and lateral portions of the femoropatellar joint capsule from both stifles of 12 mature New Zealand White rabbits were used. Specimens were divided into three treatment groups (5 watts, 10 watts, and 15 watt) and one control group using a randomized block design. Specimens were placed in a 37 degrees bath of lactated Ringer's solution and laser energy was applied using a holmium:yttrium-aluminum-garnet laser in four transverse passes across the tissue at a velocity of 2 mm/sec with the handpiece set 1.5 mm from the synovial surface. Histologic analysis revealed thermal alteration of collagen (fusion) and fibroblasts (pyknosis) at all energy densities, with higher laser energy causing significantly greater morphologic changes over a larger area (P < 0.05). Application of laser energy did not significantly alter the biochemical parameters evaluated, including type I collagen content and nonreducible crosslinks (P > 0.05). This study demonstrated that nonablative laser energy caused significant thermal damage to the joint capsular tissue in an energy-dependent fashion, but type I collagen content and nonreducible crosslinks (P > 0.05). This study demonstrated that nonablative laser energy caused significant thermal damage to the joint capsular tissue in an energy-dependent fashion, but type I Collagen content and nonreducible corsslinks were not significantly altered.

NASA Discipline Musculoskeletal↗

NASA NTRS1988

Age dependency of base modification in rabbit liver DNA

Age-related modifications of DNA bases have been observed in the liver of the New Zealand white (NZW) rabbit (Oryctolagus cuniculus), a lagomorph with a median life span in captivity of 5-7 yr. The ages of the animals studied ranged from 6 wk to 9 yr. After the DNA had been extracted from the liver cell nuclei and hydrolyzed with acid, the bases were analyzed by column chromatography with Cellulofine gels (GC-15-m). Two peaks in the chromatogram, which eluted before the four DNA bases, contained modified bases. Those materials, which were obtained in relatively large amounts from old animals, were highly fluorescent, and were shown to be crosslinked base products by mass spectrometry. The yield of crosslinked products versus rabbit age (greater than 0.5 yr) can be fitted by an exponential function (correlation coefficient: 0.76 +/- 0.09).

NASA Discipline Radiation Health↗

NASA NTRS2006

Mechanically Strong, Polymer Cross-linked Aerogels (X-Aerogels)

Aerogels comprise a class of low-density, high porous solid objects consisting of dimensionally quasi-stable self-supported three-dimensional assemblies of nanoparticles. Aerogels are pursued because of properties above and beyond those of the individual nanoparticles, including low thermal conductivity, low dielectric constant and high acoustic impedance. Possible applications include thermal and vibration insulation, dielectrics for fast electronics, and hosting of functional guests for a wide variety of optical, chemical and electronic applications. Aerogels, however, are extremely fragile materials, hence they have found only limited application in some very specialized environments, for example as Cerenkov radiation detectors in certain types of nuclear reactors, aboard spacecraft as collectors of hypervelocity particles (refer to NASA's Stardust program) and as thermal insulators on planetary vehicles on Mars (refer to Sojourner Rover in 1997 and Spirit and Opportunity in 2004). Along these lines, the X-Aerogel is a new NASA-developed strong lightweight material that has resolved the fragility problem of traditional (native) aerogels. X-Aerogels are made by applying a conformal polymer coating on the surfaces of the skeletal nanoparticles of native aerogels (see Scanning Electron Micrographs). Since the relative amounts of the polymeric crosslinker and the backbone are comparable, X-Aerogels can be viewed either as aerogels modified by the templated accumulation of polymer on the skeletal nanoparticles, or as nanoporous polymers made by remplated casting of polymer on a nanostructured framework. The most striking feature of X-Aerogels is that for a nominal 3-fold increase in density (still a ultralighweight material), the mechanical strength can be up to 300 times higher than the strength of the underlying native aerogel. Thus, X-Aerogels combine a multiple of the specific compressive strength of steel, with the the thermal conductivity of styrofoam. X-Aerogels have been demonstrated with several polymers such as polyurethanes/polyureas, epoxies and polyolefins, while crosslinking of approximately 35 different oxide aerogels yields a range of dimensionally stable, porous lightweight materials with unique combinations of structural, magnetic and optical properties. The main theme in materials development for space exploration is multifunction. For example, use of one material for thermal insulation/structural component will free weight for useful payload. In that regard, X-aerogels are evaluated at NASA for cryogenic fuel storage tanks and for spacesuits. Along the same lines, major impact fro X-Aerogels is also expected in commercial applications for thermal/acoustic insulation, in catalytic reformers and converters, in filtration membranes and membranes for fuel cells, as platforms for optical, electrical and magnetic sensors, and as lightweight structural component for aircraft and satellites.

Leventis, Nicholas↗

NASA NTRS2002

Polyfunctional fluorosilicone composition, method for making, and use

A fluorosilicone crosslinker and method for making is provided. Reaction is effected between a silanol terminated polyfluoroalkyl silicone fluid and a polyalkoxysilane in the presence of a Platinum Group Metal catalyst. The fluorosilicone crosslinker can be used in combination with a silanol terminated fluoroalkyl substituted polydiorganosiloxane to formulate a neutral, condensation curable, solvent resistant sealant.

Singh, Navjot↗

NASA NTRS1999

High Temperature Thermosets

A thermoset or network polymer is an organic material where the molecules are tied together through chemical bonds (crosslinks) and therefore they cannot move past one another. As a result, these materials exhibit a certain degree of dimensional stability. The chemical composition and the degree of crosslink density of the thermoset have a pronounced effect upon the properties. High temperature thermosets offer a favorable combination of properties that makes them attractive for many applications. Their most important features are the excellent processability particularly of the low molecular weight precusor forms, the chemical and solvent resistance and the dimensional stability. The market for high temperature thermosets will increase as new uses for them are uncovered and new thermosets with better combinations of properties are developed.

Hergenrother, Paul M.↗

NASA NTRS2009

GPS Navigation for the Magnetospheric Multi-Scale Mission

In 2014. NASA is scheduled to launch the Magnetospheric Multiscale Mission (MMS), a four-satellite formation designed to monitor fluctuations in the Earth's magnetosphere. This mission has two planned phases with different orbits (1? x 12Re and 1.2 x 25Re) to allow for varying science regions of interest. To minimize ground resources and to mitigate the probability of collisions between formation members, an on-board orbit determination system consisting of a Global Positioning System (GPS) receiver and crosslink transceiver was desired. Candidate sensors would be required to acquire GPS signals both below and above the constellation while spinning at three revolutions-per-minute (RPM) and exchanging state and science information among the constellation. The Intersatellite Ranging and Alarm System (IRAS), developed by Goddard Space Flight Center (GSFC) was selected to meet this challenge. IRAS leverages the eight years of development GSFC has invested in the Navigator GPS receiver and its spacecraft communication expertise, culminating in a sensor capable of absolute and relative navigation as well as intersatellite communication. The Navigator is a state-of-the-art receiver designed to acquire and track weak GPS signals down to -147dBm. This innovation allows the receiver to track both the main lobe and the much weaker side lobe signals. The Navigator's four antenna inputs and 24 tracking channels, together with customized hardware and software, allow it to seamlessly maintain visibility while rotating. Additionally, an extended Kalman filter provides autonomous, near real-time, absolute state and time estimates. The Navigator made its maiden voyage on the Space Shuttle during the Hubble Servicing Mission, and is scheduled to fly on MMS as well as the Global Precipitation Measurement Mission (GPM). Additionally, Navigator's acquisition engine will be featured in the receiver being developed for the Orion vehicle. The crosslink transceiver is a 1/4 Watt transmitter utilizing a TDMA schedule to distribute a science quality message to all constellation members every ten seconds. Additionally the system generates one-way range measurements between formation members which is used as input to the Kalman filter. In preparation for the MMS Preliminary Design Review (PDR), the Navigator was required to pass a series of Technology Readiness Level (TRL) tests to earn the necessary TRL-6 classification. The TRL-6 level is achieved by demonstrating a prototype unit in a relevant end-to-end environment. The IRAS unit was able to meet all requirements during the testing phase, and has thus been TRL-6 qualified

Bamford, William↗

NASA NTRS2011

Effect of Graphene Addition on Shape Memory Behavior of Epoxy Resins

Shape memory polymers (SMPs) and composites are a special class of smart materials known for their ability to change size and shape upon exposure to an external stimulus (e.g. light, heat, pH, or magnetic field). These materials are commonly used for biomedical applications; however, recent attempts have been made towards developing SMPs and composites for use in aircraft and space applications. Implementing SMPs and composites to create a shape change effect in some aircraft structures could potentially reduce drag, decrease fuel consumption, and improve engine performance. This paper discusses the development of suitable materials to use in morphing aircraft structures. Thermally responsive epoxy SMPs and nanocomposites were developed and the shape memory behavior and thermo-mechanical properties were studied. Overall, preliminary results from dynamic mechanical analysis (DMA) showed that thermally actuated shape memory epoxies and nanocomposites possessed Tgs near approximately 168 C. When graphene nanofiller was added, the storage modulus and crosslinking density decreased. On the other hand, the addition of graphene enhanced the recovery behavior of the shape memory nanocomposites. It was assumed that the addition of graphene improved shape memory recovery by reducing the crosslinking density and increasing the elasticity of the nanocomposites.

Williams, Tiffany↗

NASA NTRS2013

Composite Materials With Uncured Epoxy Matrix Exposed in Stratosphere During NASA Stratospheric Balloon Flight

A cassette of uncured composite materials with epoxy resin matrixes was exposed in the stratosphere (40 km altitude) over three days. Temperature variations of -76 to 32.5C and pressure up to 2.1 torr were recorded during flight. An analysis of the chemical structure of the composites showed, that the polymer matrix exposed in the stratosphere becomes crosslinked, while the ground control materials react by way of polymerization reaction of epoxy groups. The space irradiations are considered to be responsible for crosslinking of the uncured polymers exposed in the stratosphere. The composites were cured on Earth after landing. Analysis of the cured composites showed that the polymer matrix remains active under stratospheric conditions. The results can be used for predicting curing processes of polymer composites in a free space environment during an orbital space flight.

Kondyurin, Alexey↗

NASA NTRS2014

Flexible Polyimide Aerogel Cross-linked by Poly(maleic Anhydride-alt-alkylene)

Aerogels are potential materials for aerospace applications due to their lower thermal conductivity, lighter weight, and low dielectric constant. However, silica aerogels are restricted due to their inherent fragility, hygroscopic nature, and poor mechanical properties, especially in extreme aerospace environments. In order to fit the needs of aerospace applications, developing new thermal insulation materials that are flexible, and moisture resistant is needed. To this end, we fabricated a series of polyimide aerogels crosslinked with different poly(maleic anhydride-alt-alkylene)s as seen in Scheme 1. The polyimide oligomers were made with 3,3,4,4-biphenyltetracarboxylic dianhydride (BPDA), and different diamines or diamine combinations. The resulting aerogels have low density (0.06 gcm3 to 0.16 gcm3) and high surface area (240-440 m2g). The effect of the different backbone structures on density, shrinkage, porosity, surface area, mechanical properties, moisture resistance and thermal properties will be discussed. These novel polyalkylene-imide aerogels may be potential candidates for applications such as space suit insulation for planetary surface missions, insulation for inflatable structures for habitats, inflatable aerodynamic decelerators for entry, descent and landing (EDL) operations, and cryotank insulation for advance space propulsion systems. Scheme 1. Network of polyimide aerogels crosslinked with deifferent poly(maleic anhydride).

cross-link↗