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NASA NTRS2017

Predictive Modeling of Fast-Curing Thermosets in Nozzle-Based Extrusion

This work presents an approach to modeling the dynamic spreading and curing behavior of thermosets in nozzle-based extrusions. Thermosets cover a wide range of materials, some of which permit low-temperature processing with subsequent high-temperature and high-strength working properties. Extruding thermosets may overcome the limited working temperatures and strengths of conventional thermoplastic materials used in additive manufacturing. This project aims to produce technology for the fabrication of thermoset-based structures leveraging advances made in nozzle-based extrusion, such as fused deposition modeling (FDM), material jetting, and direct writing. Understanding the synergistic interactions between spreading and fast curing of extruded thermosetting materials will provide essential insights for applications that require accurate dimensional controls, such as additive manufacturing [1], [2] and centrifugal coating/forming [3]. Two types of thermally curing thermosets -- one being a soft silicone (Ecoflex 0050) and the other being a toughened epoxy (G/Flex) -- served as the test materials in this work to obtain models for cure kinetics and viscosity. The developed models align with extensive measurements made with differential scanning calorimetry (DSC) and rheology. DSC monitors the change in the heat of reaction, which reflects the rate and degree of cure at different crosslinking stages. Rheology measures the change in complex viscosity, shear moduli, yield stress, and other properties dictated by chemical composition. By combining DSC and rheological measurements, it is possible to establish a set of models profiling the cure kinetics and chemorheology without prior knowledge of chemical composition, which is usually necessary for sophisticated mechanistic modeling. In this work, we conducted both isothermal and dynamic measurements with both DSC and rheology. With the developed models, numerical simulations yielded predictions of diameter and height of droplets, along with width and height of extruded lines cured at varied temperatures. Experimental results carried out on a goniometric platform and a nozzle-based 3D printer showed agreement with the numerical simulations. Finally, this presentation will show how the models are adaptable to the planning of tool paths and designs in additive manufacturing.

Xie, Jingjin↗

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 NTRSDate not supplied

Critical Progressive Damage Analysis Model Features for Low-Velocity Impact on Thermoset and Thermoplastic Panels

A previous verification and validation framework evaluated the ability of various progressive damage analysis (PDA) tools to predict the mechanical response and damage state in post-buckled stiffened aerospace structures composed of fiber-reinforced thermoset composite materials. Herein, the ability of PDA tools to predict damage in thermoplastic composite materials subject to low-velocity impact (LVI) loading has been assessed. LVI tests and analyses have been conducted for similar panels, comprising thermoset or thermoplastic composite materials. Preliminary test/analysis correlations revealed that using the same combination of PDA model features and finite element model-building guidelines for the thermoset and thermoplastic LVI specimens resulted in underprediction of matrix crack lengths and delaminated area in the thermoplastic analyses despite yielding good correlations for the thermoset specimens. In this paper, the quality of the test/analysis correlations for analyses of thermoplastic LVI specimens performed with different combinations of PDA model features using the NASA CompDam material model are presented. Model features that were assessed in terms of effect on the quality of the test/analysis correlation include the representation of damageable interfaces, residual thermal stresses, and fiber damage.

Frank Leone↗

NASA NTRSDate not supplied

Critical Progressive Damage Analysis Model Features for Low-Velocity Impact on Thermoset and Thermoplastic Panels

Frank Leone↗

NASA NTRSDate not supplied

In-situ Lunar Launch and Landing Pad Construction with Regolith-Thermoset Polymer Composite Materials

Lunar launch and landing pads are necessary to mitigate risks to lander/ascent vehicles and surrounding surface assets from rocket plume ejected regolith. The current state of the art of landing and launching from the lunar surface is to land/launch on unprepared regolith surfaces. Though this has been a relatively successful approach, significant risks exist for the Artemis Program due to higher thrust levels leading to increased ejecta and cratering, presence of co-located assets in the ejecta path, and potential strict surface levelness requirements. Regolith-thermoset polymer composite materials were developed and evaluated for off Earth launch and landing pad applications. Performance under hot fire conditions was assessed for two simulated Starship lunar launch/landing environments, one targeting thermal conditions and the second targeting pressure conditions. Paver test articles were prepared at 20% and 11% polymer mass fractions. Sintered paver test articles were prepared with 20% polymer grouting filling the seams between pavers. Though significant erosion was experienced during the more extreme thermal testing conditions, all test articles successfully mitigated regolith ejecta from plume effects. A concept for preparing and emplacing the materials was developed and tested in laboratory conditions. The testing evaluated the feasibility of using twin and single screw extruder technology to mix, convey and deposit materials. Both the twin and single screw extruders were capable of processing and extruding the composite with a maximum of 90% mass fraction of regolith achieved by the twin screw extruder.A primary risk for application of regolith-thermoset polymer composites as lunar launch/landingpad is the mass of polymer required to be landed on the moon. Calculations were performed that show that a 100 m diameter, 0.025 m thick pad with polymer mass fraction of 15% will require a payload mass of 72 mt to the Lunar surface. This is below the planned Starship payload capacity to the lunar surface of 100 mt. The regolith-thermoset polymer composite based construction approach proved feasibility in three critical areas: performance under launch/landing conditions, demonstration of a mixing and depositing strategy, and fitting within the planned lunar payload capacity. It is recommended that materials and systems be developed to TRL 6 for a small-scale lunar demonstration of emplacement of a launch/landing pad via a CLPS mission to support Artemis Program roadmap gap closure activities.

ISRU↗

NASA NTRS1984

Chemoviscosity modeling for thermosetting resins - I

A new analytical model for chemoviscosity variation during cure of thermosetting resins was developed. This model is derived by modifying the widely used WLF (Williams-Landel-Ferry) Theory in polymer rheology. Major assumptions involved are that the rate of reaction is diffusion controlled and is linearly inversely proportional to the viscosity of the medium over the entire cure cycle. The resultant first order nonlinear differential equation is solved numerically, and the model predictions compare favorably with experimental data of EPON 828/Agent U obtained on a Rheometrics System 4 Rheometer. The model describes chemoviscosity up to a range of six orders of magnitude under isothermal curing conditions. The extremely non-linear chemoviscosity profile for a dynamic heating cure cycle is predicted as well. The model is also shown to predict changes of glass transition temperature for the thermosetting resin during cure. The physical significance of this prediction is unclear at the present time, however, and further research is required. From the chemoviscosity simulation point of view, the technique of establishing an analytical model as described here is easily applied to any thermosetting resin. The model thus obtained is used in real-time process controls for fabricating composite materials.

Hou, T. H.↗

NASA NTRS1988

Cellular thermosetting fluoropolymers and process for making them

Thermosetting fluoropolymer foams are made by mixing fluid from thermosetting fluoropolymer components having a substantial fluoride content, placing the mixture in a pressure tight chamber, filling the chamber with a gas, at a relatively low pressure, that is unreactive with the fluoropolymer components, allowing the mixture to gel, removing the gelled fluoropolymer from the chamber and therafter heating the fluoropolymer at a relatively low temperature to simultaneously cure and foam the fluoropolymer. The resulting fluoropolymer product is closed celled with the cells storing the gas employed for foaming. The fluoropolymer resins employed may be any thermosetting fluoropolymer including fluoroepoxies, fluoropolyurethanes and fluoroacrylates.

Lee, Sheng Y.↗

NASA NTRS1989

Cellular thermosetting fluorodiepoxide polymers

Thermosetting fluoropolymer foams are made by mixing fluid form thermosetting fluoropolymer components having a substantial fluorine content, placing the mixture in a pressure tight chamber, filling the chamber with a gas, at relatively low pressure, that is unreactive with the fluoropolymer components, allowing the mixture to gel, removing the gelled fluoropolymer from the chamber and thereafter heating the fluoropolymer at a relatively low temperature to simultaneously sure and foam the fluoropolymer. The resulting fluoropolymer product is closed celled with the cells storing the gas employed for foaming. The fluoropolymer resins employed may be any thermosetting fluoropolymer including fluoroepoxies, fluoropolyurethanes and fluoroacrylates.

Lee, Sheng Y.↗

NASA NTRS1992

Static and dynamic strain energy release rates in toughened thermosetting composite laminates

In this work, the static and dynamic fracture properties of several thermosetting resin based composite laminates are presented. Two classes of materials are explored. These are homogeneous, thermosetting resins and toughened, multi-phase, thermosetting resin systems. Multi-phase resin materials have shown enhancement over homogenous materials with respect to damage resistance. The development of new dynamic tests are presented for composite laminates based on Width Tapered Double Cantilevered Beam (WTDCB) for Mode 1 fracture and the End Notched Flexure (ENF) specimen. The WTDCB sample was loaded via a low inertia, pneumatic cylinder to produce rapid cross-head displacements. A high rate, piezo-electric load cell and an accelerometer were mounted on the specimen. A digital oscilloscope was used for data acquisition. Typical static and dynamic load versus displacement plots are presented. The ENF specimen was impacted in three point bending with an instrumented impact tower. Fracture initiation and propagation energies under static and dynamic conditions were determined analytically and experimentally. The test results for Mode 1 fracture are relatively insensitive to strain rate effects for the laminates tested in this study. The test results from Mode 2 fracture indicate that the toughened systems provide superior fracture initiation and higher resistance to propagation under dynamic conditions. While the static fracture properties of the homogeneous systems may be relatively high, the apparent Mode 2 dynamic critical strain energy release rate drops significantly. The results indicate that static Mode 2 fracture testing is inadequate for determining the fracture performance of composite structures subjected to conditions such as low velocity impact. A good correlation between the basic Mode 2 dynamic fracture properties and the performance is a combined material/structural Compression After Impact (CAI) test is found. These results underscore the importance of examining rate-dependent behavior for determining the longevity of structures manufactured from composite materials.

Cairns, Douglas S.↗

NASA NTRS2003

Optimal Substrate Preheating Model for Thermal Spray Deposition of Thermosets onto Polymer Matrix Composites

High velocity oxy-fuel (HVOF) sprayed, functionally graded polyimide/WC-Co composite coatings on polymer matrix composites (PMC's) are being investigated for applications in turbine engine technologies. This requires that the polyimide, used as the matrix material, be fully crosslinked during deposition in order to maximize its engineering properties. The rapid heating and cooling nature of the HVOF spray process and the high heat flux through the coating into the substrate typically do not allow sufficient time at temperature for curing of the thermoset. It was hypothesized that external substrate preheating might enhance the deposition behavior and curing reaction during the thermal spraying of polyimide thermosets. A simple analytical process model for the deposition of thermosetting polyimide onto polymer matrix composites by HVOF thermal spray technology has been developed. The model incorporates various heat transfer mechanisms and enables surface temperature profiles of the coating to be simulated, primarily as a function of substrate preheating temperature. Four cases were modeled: (i) no substrate preheating; (ii) substrates electrically preheated from the rear; (iii) substrates preheated by hot air from the front face; and (iv) substrates electrically preheated from the rear and by hot air from the front.

Ivosevic, M.↗

NASA NTRS2016

Reversible Thermoset Adhesives

Embodiments of a reversible thermoset adhesive formed by incorporating thermally-reversible cross-linking units and a method for making the reversible thermoset adhesive are provided. One approach to formulating reversible thermoset adhesives includes incorporating dienes, such as furans, and dienophiles, such as maleimides, into a polymer network as reversible covalent cross-links using Diels Alder cross-link formation between the diene and dienophile. The chemical components may be selected based on their compatibility with adhesive chemistry as well as their ability to undergo controlled, reversible cross-linking chemistry.

Mac Murray, Benjamin C.↗

NASA NTRS1974

Isothermal transitions of a thermosetting system

A study of the curing reactions of a cycloaliphatic epoxy resin/anhydride system by torsional braid analysis showed the existence of two critical isothermal temperatures - namely, the maximum glass transition temperature of the thermoset system and the glass transition temperature of the material at its gel point. Two rheologically active kinetic transitions occur during isothermal cure which correspond to gelation and vitrification. Three types of isothermal behavior occur. Methods for determining the time to gel and the time to vitrify, and also the two above-mentioned critical isothermal temperatures, have been developed. The time to gel obeyed the Arrhenius relationship, whereas the time to vitrify passed through a minimum. Application of these results to thermosetting systems in general is discussed in terms of the influence of molecular structure on the values of the critical isothermal temperatures.

Gillham, J. K.↗

NASA NTRS1982

Capillary rheometry for thermosets

Capillary rheometry is effectively used with thermosets. Most important is providing a uniform temperature in the barrel. This was successfully accomplished by using a circulating hot oil system. Standard capillary rheometry methods provide the dependence of thermoset apparent viscosity on shear rate, temperature and time. Such information is very useful in evaluating resin processability and in setting preliminary fabrication conditions.

Malguarnera, S. C.↗

NASA NTRS1985

NASA/aircraft industry standard specification for graphite fiber toughened thermoset resin composite material

A standard specification for a selected class of graphite fiber/toughened thermoset resin matrix material was developed through joint NASA/Aircraft Industry effort. This specification was compiled to provide uniform requirements and tests for qualifying prepreg systems and for acceptance of prepreg batches. The specification applies specifically to a class of composite prepreg consisting of unidirectional graphite fibers impregnated with a toughened thermoset resin that produce laminates with service temperatures from -65 F to 200 F when cured at temperatures below or equal to 350 F. The specified prepreg has a fiber areal weight of 145 g sq m. The specified tests are limited to those required to set minimum standards for the uncured prepreg and cured laminates, and are not intended to provide design allowable properties.

Source record↗

NASA NTRS1985

Chemoviscosity modeling for thermosetting resins, 2

A new analytical model for simulating chemoviscosity of thermosetting resin was formulated. The model is developed by modifying the Williams-Landel-Ferry (WLF) theory in polymer rheology for thermoplastic materials. By assuming a linear relationship between the glass transition temperature and the degree of cure of the resin system under cure, the WLF theory can be modified to account for the factor of reaction time. Temperature dependent functions of the modified WLF theory constants were determined from the isothermal cure data of Lee, Loos, and Springer for the Hercules 3501-6 resin system. Theoretical predictions of the model for the resin under dynamic heating cure cycles were shown to compare favorably with the experimental data reported by Carpenter. A chemoviscosity model which is capable of not only describing viscosity profiles accurately under various cure cycles, but also correlating viscosity data to the changes of physical properties associated with the structural transformations of the thermosetting resin systems during cure was established.

Hou, T. H.↗

NASA NTRS1985

Chemoviscosity modeling for thermosetting resins

A chemoviscosity model, which describes viscosity rise profiles accurately under various cure cycles, and correlates viscosity data to the changes of physical properties associated with structural transformations of the thermosetting resin system during cure, was established. Work completed on chemoviscosity modeling for thermosetting resins is reported.

Tiwari, S. N.↗

NASA NTRS1987

Studies on chemoviscosity modeling for thermosetting resins

A new analytical model for simulating chemoviscosity of thermosetting resins has been formulated. The model is developed by modifying the well-established Williams-Landel-Ferry (WLF) theory in polymer rheology for thermoplastic materials. By introducing a relationship between the glass transition temperature Tg(t) and the degree of cure alpha(t) of the resin system under cure, the WLF theory can be modified to account for the factor of reaction time. Temperature dependent functions of the modified WLF theory constants C sub 1 (t) and C sub 2 (t) were determined from the isothermal cure data. Theoretical predictions of the model for the resin under dynamic heating cure cycles were shown to compare favorably with the experimental data. This work represents progress toward establishing a chemoviscosity model which is capable of not only describing viscosity profiles accurately under various cure cycles, but also correlating viscosity data to the changes of physical properties associated with the structural transformation of the thermosetting resin systems during cure.

Bai, J. M.↗

NASA NTRS1990

Supportability evaluation of thermoplastic and thermoset composites

Nearly 300 advanced composite components manufactured by Northrop Corporation are flying on U.S. Air Force and U.S. Navy supersonic aircraft as part of a three-year Air Force/Navy/Northrop supportability evaluation. Both thermoplastic and high-temperature thermoset composites were evaluated for their in-service performance on 48 USAF and Navy F-5E fighter and USAFT-38 trainer aircraft in the first large-scale, long-term maintenance evaluation of these advanced materials. Northrop manufactured four types of doors for the project-avionics bay access, oil fill, inlet duct inspection, and a main landing gear door. The doors are made of PEEK (polyetheretherketone) thermoplastic, which is tougher and potentially less expensive to manufacture than conventional composites; and 5250-3 BMI (bismaleimide) thermoset, which is manufactured like a conventional epoxy composite but can withstand higher service temperatures. Results obtained so far indicate that both the BMI and PEEK are durable with PEEK being somewhat better than BMI.

Chanani, G. R.↗