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All sourcesNASA NTRSDOE OSTI
NASA NTRS2013

Engineered Polymer Composites Through Electrospun Nanofiber Coating of Fiber Tows

Toughening and other property enhancements of composite materials are typically implemented by-modifying the bulk properties of the constituents, either the fiber or matrix materials. This often leads to difficulties in processing and higher material costs. Many composites consist of tows or yarns (thousands of individual fibers) that are either filament wound or processed into a fabric by weaving or braiding. The matrix material can be added to the tow or fabric before final processing, resulting in a prepreg material, or infused into the fiber material during final processing by a variety of methods. By using a direct electrospun deposition method to apply thermoplastic nanofiber to the surface of the tows, the tow-tow interface in the resulting composite can be modified while using otherwise conventional materials and handling processes. Other materials of interest could also be incorporated into the electrospun precursor.

toughening↗
NASA NTRS2012

Demonstration of Minimally Machined Honeycomb Silicon Carbide Mirrors

Honeycomb silicon carbide composite mirrors are made from a carbon fiber preform that is molded into a honeycomb shape using a rigid mold. The carbon fiber honeycomb is densified by using polymer infiltration pyrolysis, or through a reaction with liquid silicon. A chemical vapor deposit, or chemical vapor composite (CVC), process is used to deposit a polishable silicon or silicon carbide cladding on the honeycomb structure. Alternatively, the cladding may be replaced by a freestanding, replicated CVC SiC facesheet that is bonded to the honeycomb. The resulting carbon fiber-reinforced silicon carbide honeycomb structure is a ceramic matrix composite material with high stiffness and mechanical strength, high thermal conductivity, and low CTE (coefficient of thermal expansion). This innovation enables rapid, inexpensive manufacturing. The web thickness of the new material is less than 1 millimeter, and core geometries tailored. These parameters are based on precursor carbon-carbon honeycomb material made and patented by Ultracor. It is estimated at the time of this reporting that the HoneySiC(Trademark) will have a net production cost on the order of $38,000 per square meter. This includes an Ultracor raw material cost of about $97,000 per square meter, and a Trex silicon carbide deposition cost of $27,000 per square meter. Even at double this price, HoneySiC would beat NASA's goal of $100,000 per square meter. Cost savings are estimated to be 40 to 100 times that of current mirror technologies. The organic, rich prepreg material has a density of 56 kilograms per cubic meter. A charred carbon-carbon panel (volatile organics burnt off) has a density of 270 kilograms per cubic meter. Therefore, it is estimated that a HoneySiC panel would have a density of no more than 900 kilograms per cubic meter, which is about half that of beryllium and about onethird the density of bulk silicon carbide. It is also estimated that larger mirrors could be produced in a matter of weeks. Each cell is completely uniform, maintaining the shape of the inserted mandrel. Furthermore, the layup creates pressure that insures node bond strength. Each node is a composite laminate using only the inherent resin system to form the bond. This contrasts starkly with the other known method of producing composite honeycomb, in which individual corrugations are formed, cured, and then bonded together in a secondary process. By varying the size of the mandrels within the layup, varying degrees of density can be achieved. Typical sizes are 3/8 and 3/16 in. (approximately 10 and 5 millimeters). Cell sizes up to 1 in. (approximately 25 millimeters) have been manufactured. Similarly, the shape of the core can be altered for a flexible honeycomb structure.

Goodman, William↗
NASA NTRS2005

PETIs as High-Temperature Resin-Transfer-Molding Materials

Compositions of, and processes for fabricating, high-temperature composite materials from phenylethynyl-terminated imide (PETI) oligomers by resin-transfer molding (RTM) and resin infusion have been developed. Composites having a combination of excellent mechanical properties and long-term high-temperature stability have been readily fabricated. These materials are particularly useful for the fabrication of high-temperature structures for jet-engine components, structural components on highspeed aircraft, spacecraft, and missiles. Phenylethynyl-terminated amide acid oligomers that are precursors of PETI oligomers are easily made through the reaction of a mixture of aromatic diamines with aromatic dianhydrides at high stoichiometric offsets and 4-phenylethynylphthalic anhydride (PEPA) as an end-capper in a polar solvent such as N-methylpyrrolidinone (NMP). These oligomers are subsequently cyclodehydrated -- for example, by heating the solution in the presence of toluene to remove the water by azeotropic distillation to form low-molecular-weight imide oligomers. More precisely, what is obtained is a mixture of PETI oligomeric species, spanning a range of molecular weights, that exhibits a stable melt viscosity of less than approximately 60 poise (and generally less than 10 poise) at a temperature below 300 deg C. After curing of the oligomers at a temperature of 371 deg C, the resulting polymer can have a glass-transition temperature (Tg) as high as 375 C, the exact value depending on the compositions.

Connell, John N.↗
NASA NTRSDate not supplied

Predicting Char Yield of High-Temperature Resins

A simulation technique has been developed for predicting the char yield of organic resins during high-temperature processing. In silico methods can aid in the screening of new advanced materials for a number of important properties, but no chemistry-sensitive protocol currently exists for predicting the important experimental value of char yield. The proposed method utilizes a reactive force field (ReaxFF) to model the chemical transformation of precursor monomers into carbonized structures during three processing stages: ramp-up to pyrolysis temperatures (~3000 K), pyrolysis, and quenching. Achieving good agreement with experimental char yields requires continuous removal of small by-product molecules to mimic outgassing, and the application of high pressure to encourage the formation of a dense, glassy network. Six different resin chemistries were investigated: an ethynyl, a phenylethynyl, a cyanate ester, a phthalonitrile, acrylonitrile, and adamantane. These candidates represent a diverse group of precursors with respect to initial cyclic content, presence of heteroatoms, and types of reactive groups. The protocol developed accurately predicts the relative char yield between the investigated chemistries and provides quantitative agreement with experimental values, especially for high char yield resins. Several simulated properties of the carbonized structures are compared with experimental results, including outgassing products, morphology of the final chemical configurations, cyclic content, and mechanical properties.

polymer simulations, molecular dynamics↗
NASA NTRS1993

Property enchancement of polyimide films by way of the incorporation of lanthanide metal ions

Lanthanide metal ions were incorporated into the polyimide derived from 2,2-bis(3,4-dicarboxyphenyl) hexafluoropropane dianhydride (6FDA) and 1,3-bis(aminophenoxy) benzene (APB) in an attempt to produce molecular level metal-polymer composites. The lanthanide series of metal ions (including aluminum, scandium, and yttrium) provide discrete and stable metal ions in the 3+ oxidation state. Throughout the series there is a uniform variation in ionic size ranging from 50 pm for aluminum to a maximum of 103.4 pm for cerium and gradually decreasing again to 84.8 pm for lutetium. The high charge-to-size ratio for these ions as well as the ability to obtain large coordination numbers makes them excellent candidates for interacting with the polymer substructure. The distinct lack of solubility of simple lanthanide salts such as the acetates and halides has made it difficult to obtain metal ions distributed in the polymer framework as discrete ions or metal complexes rather than microcomposites of metal clusters. (Lanthanum nitrates are quite soluble, but the presence of the strongly oxidizing nitrate ion leads to serious degradation of the polymer upon thermal curing. This work was successful at extending the range of soluble metals salts by using chelating agents derived from the beta-diketones dipivaloylmethane, dibenzoylmethane, trifluoroacetylacetone, and hexafluoroacetylacetone. Metal acetates which are insoluble in dimethylacetamide dissolve readily in the presence of the diketones. Addition of the polyimide yields a homogeneous resin which is then cast into a clear film. Upon curing clear films were obtained with the dibenzoylmethane and trifluoroacetylacetone ligands. The dipavaloylmethane precipitates the metal during the film casting process, and hexafluoroacetylacetone gives cured films which are deformed and brittle. These clear films are being evaluated for the effect of the metal ions on the coefficient of thermal expansion, resistance to atomic oxygen, and on selective gas permeability. Much more commonly than above, polyimide films are prepared by casting the film as the poly(amic acid) precursor which is then converted to the imidized form during the thermal cure cycle. Very limited success was achieved in the past in adding lanthanide metal ions to the amide precursors because of gellation and lack of solubility. With the use of the diketone ligands cited above, the solubility and gellation problems were overcome. However, the films after curing were clear but unacceptably brittle. Attempts to overcome this cure embrittlement problem are in progress.

Thompson, David W.↗
NASA NTRS1997

Diamines Containing Pendent Phenylethynyl Groups

Controlled molecular weight imide oligomers and co-oligomers containing pendent phenylethynyl groups (PEPIs) and endcapped with nonreactive or phenylethynyl groups have been prepared by the cyclodehydration of the precursor amide acid oligomers or co-oligomers containing pendent phenylethynyl groups and endcapped with nonreactive or phenylethynyl groups. The amine terminated amide acid oligomers or co-oligomers are prepared from the reaction of dianhydride(s) with an excess of diamine(s) and diamine containing pendent phenylethynyl groups and subsequently endcapped with a phenylethynyl phthalic anhydride or monofunctional anhydride. The anhydride terminated amide acid oligomers and co-oligomers are prepared from the reaction of diamine(s) and diamine containing pendent phenylethynyl group(s) with an excess of dianhydride(s) and subsequently endcapped with a phenylethynyl amine or monofunctional amine. The polymerizations are carried out in polar aprotic solvents such as and N,N-dimethylacetamide under nitrogen at room temperature. The amide acid oligomers or co-oligomers are subsequently cyclodehydrated either thermally or chemically to the corresponding imide oligomers. The polymers and copolymers prepared from these materials exhibit a unique and unexpected combination of properties that includes higher glass transition temperatures after curing and higher retention of neat resin, adhesive and carbon fiber reinforced mechanical properties at temperatures up to 204 C under wet conditions without sacrificing melt flow behavior and processability as compared to similar materials. These materials are useful as adhesives, coatings, films, moldings, and composite matrices.

Connell, John W.↗
NASA NTRS2019

NASA Centennial Challenge: 3D Printed Habitat, Phase 3 Final Results

NASA's Centennial Challenges program uses prize competitions with the goal of accelerating innovation in the aerospace industry. Competitions in the Centennial Challenges portfolio have previously focused on advancements in space robotics, regolith excavation, bio-printing, astronaut suit design, small satellites, and solar-powered vehicles. NASA's Three Dimensional (3D) Printed Habitat Centennial Challenge represents a partnership between NASA and the non-profit partner: Bradley University, with co-sponsors Caterpillar, Bechtel, Brick and Mortar Ventures, the American Concrete Institute, and the United States Army Corps of Engineers (USACE) Engineer Research and Development Center (ERDC) to spur development in automated additive construction technologies. The challenge asks teams to design and construct a scaled and simulated Martian habitat using indigenous materials and large scale 3D automated printing systems. Phase 1 of the competition, held in 2015, was an architectural design competition for habitat concepts that could be 3D printed. Phase 2, completed in 2017, asked teams to develop feedstocks from indigenous materials and hydrocarbon polymer recyclables, and demonstrate automated printing systems to manufacture these feedstocks into test specimens to assess mechanical strength. This paper will discuss the Phase 3 competition, focusing on technology outcomes that can potentially be infused into both terrestrial and planetary construction applications. The Phase 3 competition was divided into two sub-competitions: 1) virtual construction, where teams created a high fidelity building information model (BIM) of their 3D-printed habitat design and 2) the construction competition, which required teams to 3D print a structural foundation and subject materials samples to freeze/thaw testing and impact testing (level 1), produce a habitat element and complete a hydrostatic test (level 2), and additively manufacture a 1:3 scale habitat onsite in a head to head competition at Caterpillar, inc.'s Edwards Demonstration & Learning Center near Peoria, Illinois over the course of three days (level 3). While the Phase 2 competition focused primarily on the development of novel feedstocks and robotic printing systems, Phase 3 emphasized the scale-up of these systems and autonomous operation (demonstrating the capability to operate systems on precursor missions prior to the arrival of crew, or terrestrially in field operation settings where human tending of a manufacturing system may be limited). The Phase 3 virtual construction levels yielded a number of novel habitat designs, including both modular habitats and vertically-oriented habitat concepts. The Phase 3 construction competition also challenged teams to autonomously place penetrations and interfacing elements in additively manufactured structures. The paper will emphasize potential applications for the new materials and technologies developed under the umbrella of the competition within NASA's portfolio and in Earth-based applications such as disaster response and infrastructure improvement.

Construction↗
NASA NTRS2019

Nasa Centennial Challenge: Three Dimensional (3d) Printed Habitat, Phase 3

NASA's Centennial Challenges program uses prize competitions with the goal of accelerating innovation in the aerospace industry. Competitions in the Centennial Challenges portfolio have previously focused on advancements in space robotics, regolith excavation, bio-printing, astronaut suit design, small satellites, and solar-powered vehicles. NASA's Three Dimensional (3D) Printed Habitat Centennial Challenge represents a partnership between NASA and the non-profit partner: Bradley University, with co-sponsors Caterpillar, Bechtel, Brick and Mortar Ventures, the American Concrete Institute, and the United States Army Corps of Engineers (USACE) Engineer Research and Development Center (ERDC) to spur development in automated additive construction technologies. The challenge asks teams to design and construct a scaled and simulated Martian habitat using indigenous materials and large scale 3D automated printing systems. Phase 1 of the competition, held in 2015, was an architectural design competition for habitat concepts that could be 3D printed. Phase 2, completed in 2017, asked teams to develop feedstocks from indigenous materials and hydrocarbon polymer recyclables, and demonstrate automated printing systems to manufacture these feedstocks into test specimens to assess mechanical strength. This paper will discuss the Phase 3 competition, focusing on technology outcomes that can potentially be infused into both terrestrial and planetary construction applications. The Phase 3 competition was divided into two sub-competitions: 1) virtual construction, where teams created a high fidelity building information model (BIM) of their 3D-printed habitat design and 2) the construction competition, which required teams to 3D print a structural foundation and subject materials samples to freeze/thaw testing and impact testing (level 1), produce a habitat element and complete a hydrostatic test (level 2), and additively manufacture a 1:3 scale habitat onsite in a head to head competition at Caterpillar, inc.'s Edwards Demonstration & Learning Center near Peoria, Illinois over the course of three days (level 3). While the Phase 2 competition focused primarily on the development of novel feedstocks and robotic printing systems, Phase 3 emphasized the scale-up of these systems and autonomous operation (demonstrating the capability to operate systems on precursor missions prior to the arrival of crew, or terrestrially in field operation settings where human tending of a manufacturing system may be limited). The Phase 3 virtual construction levels yielded a number of novel habitat designs, including both modular habitats and vertically-oriented habitat concepts. The Phase 3 construction competition also challenged teams to autonomously place penetrations and interfacing elements in additively manufactured structures. The paper will emphasize potential applications for the new materials and technologies developed under the umbrella of the competition within NASA's portfolio and in Earth-based applications such as disaster response and infrastructure improvement.

Centennial challenge↗
NASA NTRSDate not supplied

Organic-rich fluids in Pluto’s interior—A source of cryovolcanic activity

The highly variegated surface of Pluto revealed by the New Horizons spacecraft is composed of both volatile ices (N2, CH4, CO) and H2O ice, all of which are intrinsically colorless. The colors on Pluto reveal a non-ice component generally acknowledged to be a refractory complex organic material (tholins) produced by photolysis in the planet’s atmosphere [1], and by photolysis and radiolysis of the surface ices [2-4]. These processes have produced a range of colors from pale yellow to red to brown, and result in a variation of a factor of 10in albedo across the surface. Tholins are disordered polymer-like materials made of repeating chains of linked subunits and complex combinations of functional groups containing carbon. Nitrogen, oxygen, and other elements can be substituted in both the aliphatic and aromatic subunits. The detection of the spectral absorption of an ammoniated compound associated with surface exposures of red-colored H2O ice (herein, RAW) in the LEISA spectral mapping data from New Horizons suggests that a third source of a colored material is ejected from Pluto’s interior as a water-rich fluid(cryomagma) that rapidly freezes at the low temperature (~40K) of the surface [5,6]. The ammoniated compound is thought to be an ammonia hydrate or an ammoniated salt; the spectral data cover a limited wavelength range, resulting in ambiguity in the identification of the form of the ammonia. The distribution of RAW in the vicinity of tectonically stressed and deformed geological structures, particularly graben (fossae), is seen as the result of both fluid effusion and fountaining ejection of cryoclastic materials in Pluto’s Virgil Fossae region [5,6]. RAW is seen elsewhere on Pluto, both in association with graben complexes and on broad expanses of old surface, but primarily in zones of tectonic stress. The nature of the putative subsurface fluid is unknown, but it must have existed at relatively shallow depths such that the graben faulting could reach it. Geochemical modeling of fluids in the interiors of small planetary bodies in the outer Solar System[7] shows that ammonia-bearing H2O in contact with rock and metal components produce a rich chemical soup, including gases that can, in principle, help propel the fluid from shallow reservoirs through crustal fractures to reach the surface. An organic component of the fluid cryomagma is predicted to originate from thermal processing of the components [ref] and may be an example of one-pot synthesis of such complexes as amino acid precursors [ref].

Dale P Cruikshank↗