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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Reduced graphene oxide catalytically enhances the rate of cyanate ester curing under variable frequency microwave heating

Here, the curing of Lonza Primaset PT-30 novolac cyanate ester resin and EPON 826 bisphenol-A diglycidyl ether were investigated using convective thermal heating and variable frequency microwave (VFM) heating. The addition of 1 part per hundred reduced graphene oxide (r-GO) to PT-30 novolac cyanate ester increased the VFM cure rate compared to thermal heating. Curing it at 160°C for 240 min with VFM heating resulted in a 55% degree of cure compared to a 26% degree of cure with thermal heating. This observed VFM rate enhancement is due to selective microwave heating of the r-GO particles in the resin resulting in increased r-GO catalytic activity toward cyanate ester curing. It is both a thermal and catalytic effect, the latter of which is absent when r-GO is added to a bisphenol-A diglycidyl ether resin with o-phenylenediamine hardener. Impurities present in the PT-30 matrix do not appear to contribute to its overall cure kinetics, nor do they participate in the observed VFM rate enhancement.

36 MATERIALS SCIENCE↗
NASA NTRS2016

Cyanate Ester and Phthalonitrile Impregnated Carbon Ablative TPS

Phenolic resin has extensive heritage as a TPS (Thermal Protection Systems) material, however, alternative resin systems such as Cyanate Ester and Phthalonitrile may offer improved performance compared to state-of-the-art phenolic resin. These alternative resin systems may have higher char yield, higher char strength, lower thermal conductivity and improved mechanical properties. In current work at NASA Ames alternative resin systems were uniformly infused into fibrous substrates and preliminary properties characterized. The density of the cyanate ester infused in fibrous substrate ranged from 0.25-0.3 grams per cubic centimeter compared to PICA (Phenolic resin impregnated carbon ablative) having a density of approximately 0.25 grams per cubic centimeter. The density of Phthalonitrile varies from 0.22-0.25 grams per cubic centimeter. Initial formulations of these new resin systems were recently tested at the LARC HyMETs (Hypersonic Materials Environmental Test System) facility to evaluate their performance and data such as back face temperature, char yield, and recession are compared to PICA. Cyanate Ester and Phthalonitrile impregnated carbon ablative samples showed comparable performance to phenolic resin impregnated carbon ablative samples.

Polymer↗
DOE OSTI2021

High-Temperature-Performance Cyanate Ester Composites with Carboranes

Cyanate ester (CE) is an important class of materials among high-temperature performance thermosets. It is used in aerospace launch vehicles, heat sinks, booms, and trusses of satellites etc. due to its high glass transition temperatures (>220°C), excellent thermal stability, and low flammability. Current approaches to improve the thermal stability of CE include incorporation of siloxanes or phosphorus- based flame retardants (PFRs). In this work, we have explored boron-based hydroxy (PD) and epoxy (EP) functionalized carborane additives to improve the thermal properties of CE. Carborane fillers were solvent blended at various mass loadings in the resin and cured to study their effect on thermal properties. PD and EP carboranes react with CE to form iminocarbonate and oxazolidinone linkages respectively. Cure kinetics studies at different wt% loadings explained that carboranes catalyze the curing reaction by reducing curing activation energy by about 54% and 26% for 10 wt% loadings of PD and EP carboranes respectively. In addition, carborane-filled cyanate ester (CE) nanocomposites demonstrate an exceptionally high thermal stability as compared to the pristine resin in air and inert environment. Our thermogravimetric analysis (TGA) experiments show that the ultimate char yield of the resin can be increased from 0% to as high as 76% and 82% with 30 wt% PD and EP carborane loading respectively at 1000 °C in air. The initial degradation temperature T d;5 of the composites decreased with increasing carborane loadings in both air and argon. For instance, T d;5 for CE was 465 and 471.6 °C in argon and air while that for P20 was 437.4 and 452.1 °C. Modulated TGA studies gave evidence of the effect of carboranes on degradation kinetics and the mechanism of the resin in air and inert environment. The effect of bonding between carboranes and CE at various loadings on the thermal expansion of the matrix was also studied using Thermomechanical Analyzer (TMA). PD carborane reduced the T g for P20 to about 225 °C while CE had T g >350 °C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1991

Rubber-toughened cyanate composites - Properties and toughening mechanism

Earlier work by Young et al. (1990) has shown that Dow experimental cyanate ester resin XU71787.02 is readily toughenable by rubber. A particularly effective rubber for this purpose is an experimental core-shell rubber which toughens the polymer by inducing shear yielding. This paper describes an investigation into the toughening mechanism in the corresponding carbon-fiber composite systems and the effect of fibers on composite properties. Resin-fiber interfacial shear strengths have been successfully correlated to the compressive strengths after impact and other key properties of composites based on rubber-toughened cyanate and several carbon fibers. The differences in the properties are explained by the difference in the functioning of the rubber particles during the fracture process.

Yang, P. C.↗
DOE OSTI2025

Extreme Thermal Stabilization of Carborane–Cyanate Composites via B–N Dative-Bonded Boroxine Barriers

Enhancing the thermal stability of cyanate ester (CE) resins is crucial for high-temperature aerospace applications. This study elucidates the degradation mechanisms of CE composites reinforced with carborane additives, focusing on the formation of boron–nitrogen (B–N) dative bonds and their role in improving thermal resistance. Using thermogravimetric analysis, we examined char formation and evolved gases at multiple degradation stages. Reaction sequences and char products were characterized via Fourier transform infrared spectroscopy (FTIR), solid-state 13C and 11B NMR, and evolved gas analysis using mass spectrometry and FTIR. The solid-state 11B NMR was instrumental in detecting various boron oxidation states and the formation of B–N dative bonds during decomposition. These bonds facilitate cross-linking in the char phase, enhancing material integrity at elevated temperatures. However, in inert environments, the volatility of boron additives like carborane limits their effectiveness. These findings advance the understanding of CE composite degradation mechanisms and offer critical insights for developing high-temperature-resistant materials for aerospace applications.

Fourier transform infrared spectroscopy↗
DOE OSTI2024

MOLLER Spectrometer Magnet Design With Measured Mechanical Properties of Irradiated S2-Glass Reinforced Cyanate Ester Resin at Elevated Temperature

Here, the aim of this study was to retire the risk of maintaining the integrity of S2-glass reinforced CTD-403 (a cyanate ester resin) that is exposed to radiation and elevated temperature over the life of the measurement of a lepton–lepton electroweak reaction (MOLLER) experiment in experimental Hall A at Jefferson Lab, Newport News, VA. In this article, the shear strength and flexural modulus of irradiated S2-glass reinforced CTD-403 specimens were measured at 65 °C (the magnets are to operate at less than 65 °C) under two scenarios: vacuum and gaseous nitrogen. The testing method is the short-beam shear (SBS) test according to ASTM D2344. The specimens were exposed to neutrons and gamma rays up to 124 MGy. The results show that specimens have excellent resistance against radiation, only 23% degradation of apparent shear strength with 124 MGy at 65 °C under vacuum. At the highest dose areas of the coils, tungsten plates are used to reduce the radiation dose to the resin system. The conclusion is that S2-glass reinforced CTD-403 is well-suited for electrical insulation of MOLLER magnets.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Photoelectron Spectroscopy and Theoretical Study on Monosolvated Cyanate Analogue Clusters ECX-· Sol (ECX- = NCSe-, AsCSe- and AsCS-; Sol = H2O, CH3CN)

Six monosolvated cyanate analogue clusters ECX-?Sol (ECX– = NCSe-, AsCSe-, and AsCS-; Sol = H2O and CH3CN) were investigated using negative ion photoelectron spectroscopy (NIPES). NIPES experiments show that these clusters possess overall similar spectra compared to their respective isolated ECX- anions but shift to higher electron binding energy with solvent CH3CN stabilizing the excess electrons slightly more than H2O. For the ECX-·H2O series, vertical detachment energies and their increments relative to the bare species are measured to be 3.700 / 0.370, 3.085 / 0.425, 3.085 / 0.430 eV for NCSe-, AsCSe- and AsCS-, respectively, while the corresponding values in ECX-·CH3CN series are 3.835 / 0.505, 3.145 / 0.475, and 3.135 / 0.480 eV. Ab initio electronic structure calculations indicate the excess charges located at the terminal N and Se atoms in NCSe- and migrated to the central C atom in AsCSe- and AsCS-. For NCSe-, the solvation is driven by the interactions with the two negatively charged terminal ends, while for AsCSe- and AsCS-, the solvation revolves around the interactions with the central C atom, where all the excess negative charge is concentrated. Two nearly degenerate isomers for NCSe-·H2O are identified, one forming a single strong N…H-O hydrogen bond (HB) and the other featuring a bidentate HB with two hydroxyl H atoms pointing to N and Se ends. In contrast, the negative central C atom in AsCSe-/AsCS- allows the formation of a bifurcated HB with H2O. Similar effects are observed for the acetonitrile case, in which the three H atoms of methyl group interact with the two negatively charged terminal ends in NCSe-, while prefer binding to the central negative carbon atom in AsCSe-/AsCS-. The different binding motifs derived in this work may suggest distinctly different solvation properties in NCSe- versus AsCSe-/AsCS-, with the former anion leading to asymmetric solvation at the N end of the solute, while the latter species creating more ‘isotropic’ solvation around the central C equatorial plane. This work was supported by U.S. Department of Energy (DOE), Office of Science, Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences, and Biosciences, and performed using EMSL, a national scientific user facility sponsored by DOE’s Office of Biological and Environmental Research and located at Pacific Northwest National Laboratory, which is operated by Battelle Memorial Institute for the DOE. The theoretical calculations were conducted on EMSL’s “Cascade” Supercomputer.

Yuan, Qinqin↗
NASA NTRS2004

Fabrication and Testing of Active and Adaptive Cyanate Ester Composite Mirrors

The objective of the NASA/Bennett Optical Research Inc. (BOR) NAS8-02008 Phase II Program, which also incorporated ideas developed under the earlier NASA NAS8-01035 Phase 1 Program, was to develop a large mirror fabrication and test facility with emphasis on producing large, light weight active and adaptive optics. A principle objective was to develop mandrels on which to make large composite graphite-filled cyanate ester mirrors, Deliverables were two of these superpolished lightweight active/adaptive optic composite mirrors, one 12" (approx.1/3 meter) in diameter and one 22" (approx.1/2 meter) in diameter. In addition optical superpolishers for mandrels up to 1.2 meters in diameter, test instruments for determining optical figure and scattered light, novel design actuators for making the composite mirrors both active and adaptive, and passive and active means for measuring actuator performance were developed at BOR. We are now installing a superpolisher capable of producing 3 meter diameter mirror/mandrels. All polishers utilize the principle of centrifugal elutriation and produce superpolished mandrels with surface microroughnesses under 1 nm rms.

Bennett, H. E.↗
NASA NTRS2006

Cryogenic Durability of a Carbon Fiber Reinforced Cyanate Ester Composite: Degree-of-Cure Effect

The James Webb Space Telescope (JWST) will be located approximately 1.5 million kilometers from Earth, producing extremely cold temperatures on the optical portion of the observatory. Specifically, the Optical Telescope Element (OTE) and Integrated Science Instrument Module (ISIM) will operate at approximately -240 C. Construction of the structural components of the OTE and ISIM require bonding dissimilar materials together, e.g. Invar-36 (an iron-nickel alloy) to a carbon fiber reinforced cyanate ester composite (CFRCE) with an epoxy adhesive. While these materials enable the cryogenic stability required for optical performance, their joint strength at these extreme conditions presents a unique design challenge. Therefore, the current study presents a detailed investigation into the optimization of cryogenic composite durability. It is demonstrated that by controlling the degree-of-cure of a laminate, one can achieve an enhanced resistance to microcracking and an improved residual strength following cryogenic cycling to -253 C.

Polis, Daniel L.↗
NASA NTRS2015

Development of an Ablative 3D Quartz / Cyanate Ester Composite for the Orion Spacecraft Compression Pad

With the successful flight test of the Orion Multipurpose Crew Vehicle last December, NASA is well on its way to sending humans into deep space with the goal of putting astronauts on Mars in the 2030s. Orion will receive some upgrades for its next launch in 2018 including a newly developed 3D Quartz Cyanate Ester composite material for the compression pad. The compression pads are 10-inches in diameter and 3-inches thick. The pucks are at 4 locations in the heat shield that serve as a part of the mechanism for holding the Crew and Service modules together during most mission phases prior to separation followed by Earth re-entry. Thus the compression pad has structural, aerothermal and thermal protection requirements.This paper describes the approach used for developing the new 3D composite, including continuous 3D weaving on an automated loom followed by resin transfer molding. Mechanical, thermal and arc jet testing of the 3D composite are also described.

Feldman, Jay↗
NASA NTRS2015

Development of an Ablative 3D Quartz / Cyanate Ester Composite for the Orion Spacecraft Compression Pad

With the successful flight test of the Orion Multipurpose Crew Vehicle last December, NASA is well on its way to sending humans into deep space with the ultimate goal of putting astronauts on Mars in the 2030s. Orion will receive some upgrades for its next launch in 2018 including a newly developed 3D quartz / cyanate ester composite material for the compression pad. Multiple pad locations in the heat shield serve as a part of the mechanism for holding the Crew and Service Modules together during most mission phases prior to separation followed by Earth re-entry of the Crew Module. Thus the compression pad must survive structural and aerothermal loads, and protect the adjascent structure and heat shield materials from over-heating.This paper describes the approach used for developing the new 3D composite, including continuous 3D weaving on an automated loom followed by resin transfer molding. Mechanical, thermal, arc jet ,and stress relaxation testing of the 3D composite are also described.

Feldman, Jay D.↗
NASA NTRS1978

New cyanate and cyanamide resins as composite matrices

The synthesis, polymerization, and laminate properties of two dicyanates, copolymers thereof, and a dicyanamide were studied. The effect of humidity aging (322 K (49 C), 95% relative humidity) and also aging at 505 K (232 C) in circulating air on the RT and elevated temperature properties of HT-S and T-300 unidirectional laminates was determined.

Hergenrother, P. M.↗
NASA NTRS2015

Ames Infusion Stories for NASA Annual Technology Report: Development of an Ablative 3D Quartz / Cyanate Ester Composite Multi-Functional Material for the Orion Spacecraft Compression Pad

Vehicles re-entering Earth's atmosphere require protection from the heat of atmospheric friction. The Orion Multi-Purpose Crew Vehicle (MPCV) has more demanding thermal protection system (TPS) requirements than the Low Earth Orbit (LEO) missions, especially in regions where the structural load passes through. The use of 2-dimensional laminate materials along with a metal insert, used in EFT1 flight test for the compression pad region, are deemed adequate but cannot be extended for Lunar return missions.

Smith, Brandon↗