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At least 19 records

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↗

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↗

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↗

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↗

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↗

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.↗

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.↗

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.↗

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↗

Graphite/Cyanate Ester Face Sheets for Adaptive Optics

It has been proposed that thin face sheets of wide-aperture deformable mirrors in adaptive-optics systems be made from a composite material consisting of cyanate ester filled with graphite. This composite material appears to offer an attractive alternative to low-thermal-expansion glasses that are used in some conventional optics and have been considered for adaptive-optics face sheets. Adaptive-optics face sheets are required to have maximum linear dimensions of the order of meters or even tens of meters for some astronomical applications. If the face sheets were to be made from low-thermal-expansion glasses, then they would also be required to have thicknesses of the order of a millimeter so as to obtain the optimum compromise between the stiffness needed for support and the flexibility needed to enable deformation to controlled shapes by use of actuators. It is difficult to make large glass sheets having thicknesses less than 3 mm, and 3-mm-thick glass sheets are too stiff to be deformable to the shapes typically required for correction of wavefronts of light that has traversed the terrestrial atmosphere. Moreover, the primary commercially produced candidate low-thermal-expansion glass is easily fractured when in the form of thin face sheets. Graphite-filled cyanate ester has relevant properties similar to those of the low-expansion glasses. These properties include a coefficient of thermal expansion (CTE) of the order of a hundredth of the CTEs of other typical mirror materials. The Young s modulus (which quantifies stiffness in tension and compression) of graphite-filled cyanate ester is also similar to the Young's moduli of low-thermal-expansion glasses. However, the fracture toughness of graphite-filled cyanate ester is much greater than that of the primary candidate low-thermal-expansion glass. Therefore, graphite-filled cyanate ester could be made into nearly unbreakable face sheets, having maximum linear dimensions greater than a meter and thicknesses of the order of a millimeter, that would satisfy the requirements for use in adaptive optics.

Bennett, Harold↗

Long Focal Length Large Mirror Fabrication System

The goals of this ambitious program are (1) to develop systems to make large superpolished optical mirrors, (2) to develop low scatter polishing techniques using centrifugal elutriation, (3) to develop a means of measuring scatter at any point on the mirror, (4) to polish a Hindle sphere to measure the optical figure of a one meter diameter convex mandrel, and (5) to fabricate low scatter, large adaptive optic graphite filled, cyanate ester replica transfer mirrors using these mandrels. Deliverables are a 30 cm diameter superpolished composite AO mirror. We fabricated a 1/3rd meter superpolished zerodur flat mandrel and with the support of our major subcontractor, Composite Mirror Applications Inc (CMA) we have demonstrated a 30 cm lightweight cyanate ester mirror with an rms microroughness between 0.6 and 0.8 nm and 8 faceplate influence function of 5 cm. The influence function was chosen to be comparable to the atmospheric correlation coefficient r(sub 0) which is about 5 cm at sea level. There was no print-thru of the graphite fibers in the cyanate ester surface (the bane of many previous efforts to use cyanate ester mirrors). Our subcontractor has devised a means for developing a 30-50 nm thick layer of graphite free pure ester resin on the surface of the mirrors. This graphite fiber filled material has a thermal expansion coefficient in the 10(exp -8) centimeter per Kelvin range (the same range of expansion coefficient as Zerodur and ULE glasses) and does not take up water and swell, so it is a nearly ideal mirror material in these areas. Unfortunately for these 0.8mm thick faceplates, the number of plies is not enough to result in isometric coverage. Isolated figure irregularities can appear, making it necessary to go to thicker faceplates. The influence function will then only approximate the length of r(sub 0), at higher altitudes or longer wavelengths. The influence function goes as the cube of the thickness, so we are now making a faceplate optimized for an infrared wavelength, possibly that used for the AO system of the Keck telescope, instead of 0.63 microns. We have polished a 55 cm diameter mandrel to better than 1/20th wave optical figure in the visible using centrifugal elutriation. CMA has just told us that it needs to retool to get optimum mirror faceplate quality in this size, so implementing the 55 cm AO mirror may be delayed somewhat. We expect to complete our 1/3 rd meter AO mirror on time using novel piezoelectric actuators with a throw of one micrometer per volt, as compared to 0.005 micrometers per volt for conventional piezoelectric actuators. We will then demonstrate its AO performance interferometrically.

Bennett, H. E.↗

Pyrolysis Rate and Yield Strength Reduction Incarbon Fiber and Glass Fiber Composites Underreentry Heating Conditions

The behavior of composite materials, specifically carbon fiber reinforced plastic (CFRP) and glass fiber reinforced plastic (GFRP), under reentry conditions poses a problem for space debris reentry risk modeling. Since these materials pyrolyze rather than melt and their different components demise at different rates, modeling their destruction to determine ground impact risk is complex. Modern spacecraft are using these materials in ever-greater quantities owing to their superior strength-to-weight characteristics, and this has required that the orbital debris community improve its understanding of how these materials demise on reentry. The NASA Orbital Debris Program Office undertook an extensive test campaign to better understand the rate at which several types of GFRP and CFRP materials pyrolyze under reentry heating conditions and how that pyrolysis affects the ultimate strength of the material. GFRP with a polyester resin (G10/FR-4) and CFRP with epoxy, cyanate ester, vinyl ester, and phenolic resins were tested. The test campaign was carried out at the Inductively Coupled Plasma (ICP) Torch Facility at the University of Texas at Austin. Because the ICP facility operates in a shirt-sleeve environment, test samples can be changed within seconds or minutes, allowing many samples to be tested in a short period. Two heat flux rates, 20 W/m2 and 30W/m2, and two oxygen concentration conditions, 0% and 2% of atmospheric, were applied to all five types of material. To measure both the char rate and the effect of pyrolysis on the ultimate material strength, two types of test were carried out for each material: a char rate test on a ~10 mm thick sample of material and an in-situ bending stress test of a ~2 mm thick sample of material. Measurements of the char rate showed very similar average pyrolysis front velocity in epoxy resin CFRP as in G10 at 3.6 mm/min and 3.4 mm/min, respectively. However, the total mass loss rate in theG10 was nearly double that of the CFRP at 3.8 g/min and 2.2 g/min, respectively. This result represented a slow ablation rate of carbon fibers in the CFRP at the temperatures encountered in low Earth orbit reentry and a comparatively rapid removal of the glass fibers in G10 due to melting and spallation. Pyrolysis front velocity was more significantly affected by the type of plastic than the type of fiber, with the cyanate ester CFRP samples displaying an average pyrolysis front velocity of only 1.9 mm/min. Similarly, the effect of thermal exposure on the ultimate strength of the material depended heavily on the type of plastic and very little on the type of fiber in the material. Epoxy, vinyl ester, and polyester resins all behaved very similarly, with complete structural failure at between 400 J/g and 600 J/g of specific absorbed heat. Phenolic and cyanate ester resins, on the other hand, displayed a change in structural properties that was only barely measurable with the current apparatus even after the maximum exposure time tested. These data are being incorporated into a numerical model of the ablation and demise of composite materials that will be used to more accurately calculate the ground casualty risk of future spacecraft.

Benton R. Greene↗

A Preliminary Investigation of the E-Beam Induced Polymerization of Maleimide and Norbornene End-capped Polyimides

A research area of high activity in connection with aerospace engineering has been the development of polymer thermosetting resins that can resist temperature as high as 300 C while maintaining adequate toughness, and providing ease of processing to enable low temperature and low cost composite fabrication methods. In order to meet such requirements, sequential interpenetrating polymer networks (IPNs) based on bismaleimide (BMI) and cyanate ester (CE) monomers were investigated. In these systems, a polycyanurate network is first formed in the presence of BMI and appropriate reactive diluent monomers and in a second step, a network based on the BMI is created in the presence of a fully formed polycyanurate network. The materials developed can be processed at relatively low temperature (less than 150 C) and with the aid of electron beam (EB) curing. Of major importance to the success of this work was the identification of a reactive diluent that improves ease of processing and has tailored reactivity to allow for the controlled synthesis of CE-BMI sequential IPNs. Based on solubility and reactivity of a number of reactive diluents, N-acryloylmorpholine (AMP) was selected as a comonomer for BMI copolymerization. A donor-acceptoreaction mechanism was suggested to explain the relative reactivity of a variety of reactive diluents towards maleimide functionality. The optimum processing parameters for the formation of the first network were determined through the study of metal catalyzed cure and hydrolysis of cyanate esters, whereas the reaction behavior for second network formation in terms of the influence of EB dose rate and temperature was elucidated through an in-situ kinetics study of maleimide and AMP copolymerization. Structure-property relationships were developed which allowed for the design of improved resin systems. In particular, appropriate network coupler possessing cyanate ester and maleimide functionality was synthesized to link the polycyanurate first network to the BMI/AMP second network and thus form linked sequential IPNs (LIPNs). Consequently, Tg as high as 370 C was achieved and a fracture toughness of 120 Joules per square meters was obtained for resin systems that possess adequately low viscosity for processing using liquid molding techniques at low temperature.

Palmese, Giuseppe R.↗

Mechanical Properties of High-Temperature Fiber-Reinforced Thermoset Composites with Plain Weave and Unidirectional Carbon Fiber Fillers

Fiber-reinforced thermoset composites are a class of materials that address the arising needs from the aerospace and hypersonic industries for high specific strength, temperature-resistant structural materials. Among the high-temperature resistant thermoset categories, phenolic triazine (PT) cyanate esters stand out thanks to their inherent high degradation temperature, glass transition temperature, and mechanical strength. Despite the outstanding properties of these thermosets, the performance of carbon fiber composites using PT cyanate esters as matrices has not been thoroughly characterized. This work evaluated PT and carbon fiber composites’ compressive properties and failure mechanisms with different fiber arrangements. A PT resin with both plain weave (PW) and non-crimped unidirectional (UD) carbon fiber mats was analyzed in this research. Highly loaded thermoset composites were obtained using process temperatures not exceeding 260 °C, and the composites proved to retain compressive strength at temperatures beyond 300 °C. Compressive testing revealed that PT composites retained compressive strength values of 50.4% of room temperature for UD composites and 61.4% for PW composites. Post-compressive failure observations of the gage section revealed that the mechanisms for failure evolved with temperature from brittle, delamination-dominant failure to shear-like failure promoted by the plastic failure of the matrix. This study demonstrated that PT composites are a good candidate for structural applications in harsh environments.

Hall, Samuel Ernesto↗

Microcracking of Materials for Space

The effect of thermal-cycling-induced microcracking in fiber-reinforced polymer matrix composites is studied. Specific attention is focused on microcrack density as a function of the number of thermal cycles, and the effect of microcracking on the dimensional stability of composite materials. Changes in laminate coefficient of thermal expansion (CTE) and laminate stiffness are of primary concern. Included in the study are materials containing four different Thornel fiber types: a PAN-based T50 fiber and three pitch-based fibers, P55, P75, and P120. The fiber stiffnesses range from 55 Msi to 120 Msi. The fiber CTE's range from -0.50 x 1O(exp -6)/degrees F to -0.80 x 10(exp -6)/degrees F. Also included are three matrix types: Fiberite's 934 epoxy, Amoco's ERL1962 toughened epoxy, and YLA's RS3 cyanate ester. The lamination sequences of the materials considered include a cross-ply configuration, [0/90](sub 2s), and two quasi-isotropic configurations, [0/+45/-45/90](sub s), and [0/+45/90/-45](sub s). The layer thickness of the materials range from a nominal 0.001 in. to 0.005 in. In addition to the variety of materials considered, three different thermal cycling temperature ranges are considered. These temperature ranges are +/-250 degrees F, +/-l5O degrees F, and +/-50 degrees F. The combination of these material and geometric parameters and temperature ranges, combined with thermal cycling to thousands of cycles, makes this one of the most comprehensive studies of thermal-cycling-induced microcracking to date. Experimental comparisons are presented by examining the effect of layer thickness, fiber type, matrix type, and thermal cycling temperature range on microcracking and its influence on the laminates. Results regarding layer thickness effects indicate that thin-layer laminates microcrack more severely than identical laminates with thick layers. For some specimens in this study, the number of microcracks in thin-layer specimens exceeds that in thick-layer specimens by more than a factor of two. Despite the higher number of microcracks in the thin-layer specimens, small changes in CTE after thousands of cycles indicate that the thin-layer specimens are relatively unaffected by the presence of these cracks compared to the thick-layer specimens. Results regarding fiber type indicate that the number of microcracks and the change in CTE after thousands of cycles in the specimens containing PAN-based fibers are less than in the specimens containing comparable stiffness pitch-based fibers. Results for specimens containing the different pitch-based fibers indicate that after thousands of cycles, the number of microcracks in the specimens does not depend on the modulus or CTE of the fiber. The change in laminate CTE does, however, depend highly on the stiffness and CTE of the fiber. Fibers with higher stiffness and more negative CTE exhibit the lowest change in laminate CTE as a result of thermal cycling. The overall CTE of these specimens is, however, more negative as a result of the more negative CTE of the fiber. Results regarding matrix type based on the +/-250 degree F temperature range indicate that the RS3 cyanate ester resin system exhibits the greatest resistance to microcracking and the least change in CTE, particularly for cycles numbering 3000 and less. Extrapolations to higher numbers of cycles indicate, however, that the margin of increased performance is expected to decrease with additional thermal cycling. Results regarding thermal cycling temperature range depend on the matrix type considered and the layer thickness of the specimens. For the ERL1962 resin system, microcrack saturation is expected to occur in all specimens, regardless of the temperature range to which the specimens are exposed. By contrast, the RS3 resin system demonstrates a threshold effect such that cycled to less severe temperature ranges, microcracking does not occur. For the RS3 specimens with 0.005 in. layer thickness, no microcracking or changes in CTE are observed in specimens cycled between +/-150 degree F or +/- 50 degree F. For the RS3 specimens with 0.002 in. layer thickness, no microcracking or changes in CTE are observed in specimens cycled between +/-50 degree F. Results regarding laminate stiffness indicate negligible change in laminate stiffness due to thermal cycling for the materials and geometries considered in this investigation. The study includes X-ray examination of the specimens, showing that cracks observed at the edge of the specimens penetrate the entire width of the specimen. Glass transition temperatures of the specimens are measured, showing that resin chemistry is not altered as a result of thermal cycling. Results are also presented based on a one-dimensional shear lag analysis developed in the literature. The analysis requires material property information that is difficult to obtain experimentally. Using limited data from the present investigation, material properties associated with the analysis are modified to obtain reasonable agreement with measured microcrack densities. Based on these derived material properties, the analysis generally overpredicts the change in laminate CTE. Predicted changes in laminate stiffness show reasonable correlation with experimentally measured values.

Brown, Timothy L.↗

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↗