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All sourcesNASA NTRSDOE OSTI
NASA NTRS1984

Variation of Resin Properties Through the Thickness of Cured Samples

It is the purpose of this work to gain knowledge of the glassy materials used as matrices in composites and to study the homogeneity resulting from the curing process. An attempt is made to link the glass transition quantitatively with the presence of a given material. Expoxy resins containing various amounts of hardener (TGDDM/DDS system) were cured in a muffle furnace at 473 K for seven hours. The glass transition temperature, T sub g versus weight minus percent of hardener in the epoxy resin were measured. A limit was rapidly reached in T sub g at only two percent hardener. Thus, the glass transition of the fully cured epoxy-amine matrix seems not much different from the epoxide-epoxide cure. The T sub g versus cure-time for the epoxide-epoxide reaction was also studied. My 720 was cured by itself in an oil bath at 473 K for different lengths of time. The T sub g was found to increase exponentially with the cure time, and a maximum T sub g of about 450 K was reached after eleven hours. The reaction was found to be inhibited by running the sample under argon.

Source record↗
NASA NTRS1987

Optimal cure cycle design of a resin-fiber composite laminate

Fibers reinforced composites are used in many applications. The composite parts and structures are often manufactured by curing the prepreg or unmolded material. The magnitudes and durations of the cure temperature and the cure pressure applied during the cure process have significant consequences on the performance of the finished product. The goal of this study is to exploit the potential of applying the optimization technique to the cure cycle design. The press molding process of a polyester is used as an example. Various optimization formulations for the cure cycle design are investigated. Recommendations are given for further research in computerizing the cure cycle design.

Hou, Jean W.↗
NASA NTRS1997

Electron Beam Cured Epoxy Resin Composites for High Temperature Applications

Electron beam curing of Polymer Matrix Composites (PMC's) is a nonthermal, nonautoclave curing process that has been demonstrated to be a cost effective and advantageous alternative to conventional thermal curing. Advantages of electron beam curing include: reduced manufacturing costs; significantly reduced curing times; improvements in part quality and performance; reduced environmental and health concerns; and improvement in material handling. In 1994 a Cooperative Research and Development Agreement (CRADA), sponsored by the Department of Energy Defense Programs and 10 industrial partners, was established to advance the electron beam curing of PMC technology. Over the last several years a significant amount of effort within the CRADA has been devoted to the development and optimization of resin systems and PMCs that match the performance of thermal cured composites. This highly successful materials development effort has resulted in a board family of high performance, electron beam curable cationic epoxy resin systems possessing a wide range of excellent processing and property profiles. Hundreds of resin systems, both toughened and untoughened, offering unlimited formulation and processing flexibility have been developed and evaluated in the CRADA program.

Janke, Christopher J.↗
NASA NTRS2004

Curing Composite Materials Using Lower-Energy Electron Beams

In an improved method of fabricating composite-material structures by laying up prepreg tapes (tapes of fiber reinforcement impregnated by uncured matrix materials) and then curing them, one cures the layups by use of beams of electrons having kinetic energies in the range of 200 to 300 keV. In contrast, in a prior method, one used electron beams characterized by kinetic energies up to 20 MeV. The improved method was first suggested by an Italian group in 1993, but had not been demonstrated until recently. With respect to both the prior method and the present improved method, the impetus for the use of electron- beam curing is a desire to avoid the high costs of autoclaves large enough to effect thermal curing of large composite-material structures. Unfortunately, in the prior method, the advantages of electron-beam curing are offset by the need for special walls and ceilings on curing chambers to shield personnel from x rays generated by impacts of energetic electrons. These shields must be thick [typically 2 to 3 ft (about 0.6 to 0.9 m) if made of concrete] and are therefore expensive. They also make it difficult to bring large structures into and out of the curing chambers. Currently, all major companies that fabricate composite-material spacecraft and aircraft structures form their layups by use of automated tape placement (ATP) machines. In the present improved method, an electron-beam gun is attached to an ATP head and used to irradiate the tape as it is pressed onto the workpiece. The electron kinetic energy between 200 and 300 keV is sufficient for penetration of the ply being laid plus one or two of the plies underneath it. Provided that the electron-beam gun is properly positioned, it is possible to administer the required electron dose and, at the same time, to protect personnel with less shielding than is needed in the prior method. Adequate shielding can be provided by concrete walls 6 ft (approximately equal to 1.8 m) high and 16 in. (approximately equal to 41 cm) thick, without a ceiling. The success of the present method depends on the use of a cationic epoxy as the matrix material in the prepreg tape, heating the prepreg tape to a temperature of 50 C immediately prior to layup, and exposing the workpiece to an electron-beam dose of approximately 2 Mrad. Experiments have shown that structures fabricated by the present method have the same mechanical properties as those of nominally identical structures fabricated by the prior method with electron beams of 3 to 4 MeV.

Byrne, Catherine A.↗
NASA NTRS2016

Development of a Fully Automated Guided Wave System for In-Process Cure Monitoring of CFRP Composite Laminates

A guided wave-based in-process cure monitoring technique for carbon fiber reinforced polymer (CFRP) composites was investigated at NASA Langley Research Center. A key cure transition point (vitrification) was identified and the degree of cure was monitored using metrics such as amplitude and time of arrival (TOA) of guided waves. Using an automated system preliminarily developed in this work, high-temperature piezoelectric transducers were utilized to interrogate a twenty-four ply unidirectional composite panel fabricated from Hexcel (Registered Trademark) IM7/8552 prepreg during cure. It was shown that the amplitude of the guided wave increased sharply around vitrification and the TOA curve possessed an inverse relationship with degree of cure. The work is a first step in demonstrating the feasibility of transitioning the technique to perform in-process cure monitoring in an autoclave, defect detection during cure, and ultimately a closed-loop process control to maximize composite part quality and consistency.

Hudson, Tyler B.↗
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 NTRS1982

The properties of novel bisimide amine cured epoxy/Celion 6000 graphite fiber composites

The study is concerned with the further development of bisimide amine cured epoxy resins first reported by Serafini et al. (1979). Attention is given to properties of the neat resins and composites made with these novel epoxy resins and Celion 6000 graphite fibers. The use of bisimide amine hardeners to cure epoxy resins causes a significant improvement in the char-forming characteristics of the cured resin. Compared to epoxy resins cured with a conventional amine, such as 4,4'-diaminodiphenylsulfone, the bisimide cured epoxies exhibit about a twofold improvement in the aerobic char yield at 800 C. The levels of moisture absorption exhibited by the bisimide amine cured epoxies were found to be considerably lower than those exhibited by state-of-the-art epoxies (0.5 wt.% versus 2.0%).

Scola, D. A.↗
NASA NTRS1986

A study of the possible effect of a thermal post cure on the mechanical properties of the 404 carbon-phenolic ring of the space shuttle solid rocket motor nozzle

Erratic pockets of erosion have occurred on the inner perimeter of the 404 rocket nozzle ring during liftoff firing. It is thought that it may be caused by pockets of volatile matter entrapped during manufacture. A thermal post cure was suggested as a possible means of outgassing such pockets, if they in fact do exist. To confirm an outgassing during a post cure and to establish a working upper temperature limit, thermal gravimetric and differential calorimetric analyses were made on a number of samples from two 404 rings supplied by the manufacturer. Continuous weight loss was observed over the temperature range explored (750 F) indicating outgassing, and a strong exothermic reaction occurs beginning about 390 F. Thus, an upper post cure temperature of 350 F is recommended. To determine the possible effect of a post cure on physical properties, the following tests will be made on matched sets of cured and post cured material: x-radiography (internal structure), linear dimensions, weight, porosity, cross ply thermal expansion, drop and double notch shear strengths, and tensional strength in the ply direction.

Giardini, A. A.↗
NASA NTRS1987

Optimal cure cycle design of a resin-fiber composite laminate

A unified computed aided design method was studied for the cure cycle design that incorporates an optimal design technique with the analytical model of a composite cure process. The preliminary results of using this proposed method for optimal cure cycle design are reported and discussed. The cure process of interest is the compression molding of a polyester which is described by a diffusion reaction system. The finite element method is employed to convert the initial boundary value problem into a set of first order differential equations which are solved simultaneously by the DE program. The equations for thermal design sensitivities are derived by using the direct differentiation method and are solved by the DE program. A recursive quadratic programming algorithm with an active set strategy called a linearization method is used to optimally design the cure cycle, subjected to the given design performance requirements. The difficulty of casting the cure cycle design process into a proper mathematical form is recognized. Various optimal design problems are formulated to address theses aspects. The optimal solutions of these formulations are compared and discussed.

Hou, Jean W.↗
NASA NTRS1992

ASRM test report: Autoclave cure process development

ASRM insulated segments will be autoclave cured following insulation pre-form installation and strip wind operations. Following competitive bidding, Aerojet ASRM Division (AAD) Purchase Order 100142 was awarded to American Fuel Cell and Coated Fabrics Company, Inc. (Amfuel), Magnolia, AR, for subcontracted insulation autoclave cure process development. Autoclave cure process development test requirements were included in Task 3 of TM05514, Manufacturing Process Development Specification for Integrated Insulation Characterization and Stripwind Process Development. The test objective was to establish autoclave cure process parameters for ASRM insulated segments. Six tasks were completed to: (1) evaluate cure parameters that control acceptable vulcanization of ASRM Kevlar-filled EPDM insulation material; (2) identify first and second order impact parameters on the autoclave cure process; and (3) evaluate insulation material flow-out characteristics to support pre-form configuration design.

Nachbar, D. L.↗
NASA NTRS2001

Electron Beam-Cure Polymer Matrix Composites: Processing and Properties

Researchers from NASA and Oak Ridge National Laboratory are evaluating a series of electron beam curable composites for application in reusable launch vehicle airframe and propulsion systems. Objectives are to develop electron beam curable composites that are useful at cryogenic to elevated temperatures (-217 C to 200 C), validate key mechanical properties of these composites, and demonstrate cost-saving fabrication methods at the subcomponent level. Electron beam curing of polymer matrix composites is an enabling capability for production of aerospace structures in a non-autoclave process. Payoffs of this technology will be fabrication of composite structures at room temperature, reduced tooling cost and cure time, and improvements in component durability. This presentation covers the results of material property evaluations for electron beam-cured composites made with either unidirectional tape or woven fabric architectures. Resin systems have been evaluated for performance in ambient, cryogenic, and elevated temperature conditions. Results for electron beam composites and similar composites cured in conventional processes are reviewed for comparison. Fabrication demonstrations were also performed for electron beam-cured composite airframe and propulsion piping subcomponents. These parts have been built to validate manufacturing methods with electron beam composite materials, to evaluate electron beam curing processing parameters, and to demonstrate lightweight, low-cost tooling options.

Wrenn, G.↗
NASA NTRS2002

Effects of Amine and Anhydride Curing Agents on the VARTM Matrix Processing Properties

To ensure successful application of composite structure for aerospace vehicles, it is necessary to develop material systems that meet a variety of requirements. The industry has recently developed a number of low-viscosity epoxy resins to meet the processing requirements associated with vacuum assisted resin transfer molding (VARTM) of aerospace components. The curing kinetics and viscosity of two of these resins, an amine-cured epoxy system, Applied Poleramic, Inc. VR-56-4 1, and an anhydride-cured epoxy system, A.T.A.R.D. Laboratories SI-ZG-5A, have been characterized for application in the VARTM process. Simulations were carried out using the process model, COMPRO, to examine heat transfer, curing kinetics and viscosity for different panel thicknesses and cure cycles. Results of these simulations indicate that the two resins have significantly different curing behaviors and flow characteristics.

Brian W Grimsley↗
NASA NTRS2006

Designing Cure Cycles for Matrix/Fiber Composite Parts

A methodology has been devised for designing cure cycles to be used in the fabrication of matrix/fiber composite parts (including laminated parts). As used here, cure cycles signifies schedules of elevated temperature and pressure as functions of time, chosen to obtain desired rates of chemical conversion of initially chemically reactive matrix materials and to consolidate the matrix and fiber materials into dense solids. Heretofore, cure cycles have been designed following an empirical, trial-and-error approach, which cannot be relied upon to yield optimum results. In contrast, the present methodology makes it possible to design an optimum or nearly optimum cure cycle for a specific application. Proper design of a cure cycle is critical for achieving consolidation of a reactive matrix/fiber layup into a void-free laminate. A cure cycle for a composite containing a reactive resin matrix usually consists of a two-stage ramp-and-hold temperature profile. The temperature and the duration of the hold for each stage are unique for a given composite material. The first, lower-temperature ramp-and hold stage is called the B stage in composite- fabrication terminology. At this stage, pressure is not applied, and volatiles (solvents and reaction by-products) are free to escape. The second, higher-temperature stage is for final forced consolidation.

Hou, Tan-Hung↗
NASA NTRSDate not supplied

Investigation of Lunar-Inspired Geopolymer Concrete Formulations Mixed and Cured in Microgravity on the International Space Station (ISS)

The research outlined in this presentation investigates the use of various lunar regolith simulants in geopolymer lunar concrete mixes mixed and cured on the International Space Station (ISS). The motivation for this work is to study the effects of gravity on the microstructure of alkali-activated materials cured with heat, and to develop materials for the construction of long-term infrastructure on the lunar surface with in-situ resource utilization (ISRU). ISRU for construction materials reduces the cost and mass of payloads related to lunar construction. The advantage of geopolymer concrete as opposed to traditional portland cement concrete is that water acts as a medium for the polymerization reaction and leaves the system throughout the process, reducing its demand. Twelve samples of lunar regolith simulant and a solution composed of sodium hydroxide and sodium silicate were sent to the ISS. The three simulants were OPRH2N, OPRL2N, and JSC-1AF, using only particles less than 53 µm in diameter to increase reactivity of the simulant. Simulant to solution ratios were determined by workability while mixing. The simulant and solution were sealed Burst Pouches® along with 2 other sealed bags to prevent material from leaking. Crew member F-14 conducted testing on the ISS by introducing the solution to the simulant in the Burst Pouch®, mixing the sample with a spatula, and then clamping the specimen in the fresh state to prevent flow inside the Burst Pouch®. These specimens were then put in a thermos heated to 80C via sealed drinking water bags to cure for 24 hours with a temperature logger. The cured specimens remained in microgravity for at least 28 days and were returned from the ISS in February 2025. The specimens were then brought to the NASA Marshall Space Flight Center (MSFC) to analyze. Material characterization consisted of conducting Micro-CT tests of entire samples in their sealed apparatus to a resolution of 25µm. 2D image slices were saved in each orthogonal direction of each specimen at a 0.03 mm step size from the 3D model to conduct analytical porosity calculations. Representative samples from each specimen were sampled to perform helium gas pycnometery and were then mounted in resin for SEM imaging, EDS, and nanoindentation. Porosity was analyzed analytically using micromechanics modelling with the assistance of the NASA Multiscale Analysis Tool (NASMAT), as well as the NASA Advanced Supercomputing (NAS) servers (V. Saseendran & N. Yamamoto, 2024). Density was measured using helium gas pycnometery and was then compared to the theoretical density for experimental porosity calculation. Due to the samples’ non-uniform shape being cured in a pouch, traditional compression and tensile strength testing could not be performed. Nanoindentation was conducted at Clarkson University to determine the microhardness and reduced modulus of elasticity. Results from flight samples can be compared to ground samples currently in DLR’s possession to determine the effect on microstructure from being mixed and cured in microgravity. This study gives further insight and understanding of geopolymer lunar concrete and its viability as a lunar construction material with ISRU.

Adam Johnson↗
NASA NTRSDate not supplied

Effect of Composition Variation on Isothermal Rapid Curing Resins for Aerospace Applications

To meet the projected demand for single-aisle composite aircraft in 2040, the production rate of these aircraft will need to increase by four to six times what is currently achievable. A composite manufacturing process with the potential to enable the targeted rates is isothermal resin infusion where infusion and cure occur at the same temperature. However, presently there is not an accepted aerospace-grade resin that can support this isothermal infusion process and maintain acceptable resin properties. Therefore, resin development initiatives have designed anionic catalyzed epoxy systems capable of isothermal infusion and rapid cure at a temperature below 100 ˚C in one hour. High-performance aerospace properties are achieved after undergoing a freestanding post-cure. The resins facilitate faster, energy efficient production cycles by reducing the time and temperature required for cure and eliminating temperature ramps typically required of materials used in the aerospace industry. This work discusses several of the developed resin systems and the impact of varying composition on rheological, thermal, and mechanical properties. Carbon fiber composites were fabricated for one composition by resin transfer molding to demonstrate the potential of these isothermal, rapid cure systems for meeting industry needs.

resin transfer molding↗
NASA NTRS2021

Porosity Detection and Localization During Composite Cure Inside an Autoclave Using Ultrasonic Inspection

Composite materials offer unique benefits in aerospace applications such as increased strength-to-weight ratio and improved fatigue properties. They are increasingly being used in major commercial aircraft programs. However, current processing methods can lead to defects in composite parts, which must be detected using post-manufacturing inspection methods. Porosity (i.e., pores, voids) is a critical defect from the cure process that is detrimental to performance of the composite part. It is therefore necessary to understand and eliminate the formation of porosity defects. At NASA Langley Research Center, an in-situ cure monitoring system was developed to detect porosity defects as they form in real-time inside an autoclave. A capability to directly detect and localize porosity within a composite during cure did not exist before. This study is focused on an elevated-temperature ultrasonic inspection system to detect porosity defects in composites during autoclave cure. The ultrasonic inspection system operated inside an autoclave within an enclosure cooled by intermittent liquid nitrogen (LN_2) injections. A high-temperature, 2.25 MHz, transducer transmitted ultrasonic waves through the tool plate and into the composite part and measured the amplitude and time of flight of the reflected waves with a 1 mm × 1 mm step size/areal resolution. Porosity was observed via the ultrasonic reflections, which experienced increased attenuation in regions of high porosity. Distinct regions of increased porosity were present due to uneven pressure across the panel, which was driven by an intentional misfit between the flat caul plate and the tapered composite panel with ply drops. The results were validated by post-cure ultrasonic inspection and micrographs. The in-situ inspection system was able to successfully provide porosity detection and localization in the tapered ply-drop panel. The successful results indicate the promise of this system for future implementation in the manufacturing of composite structures for aerospace applications.

Composites↗
NASA NTRS2021

Latent Cure Epoxy Resins for Reliable Joints in Secondary-Bonded Composite Structures

In high-performance polymer matrix composite assemblies, adhesive bonding is generally superior to mechanical fastening in structural performance and manufacturing efficiency. However, adhesive bonds are susceptible to minute levels of contamination accumulated during assembly that can lead to unpredictable, weak bonds. Current methods of measuring bond strength are all destructive mechanical tests. To overcome these challenges, redundant load paths (e.g., mechanical fasteners) are often implemented in secondary-bonded, primary-structures, which can greatly reduce structural performance. This study investigated reformulated aerospace epoxy matrix resins with stoichiometric offset to inhibit cure of the matrix resin prior to assembly. Inhibited resins can reflow and mix across the joint interface, which eliminates the material discontinuity and forms a homogenous joint with reliable fracture properties. The goal of this study was to develop and demonstrate secondary composite assemblies that are mechanically and microscopically indistinguishable from a co-cured composite joint. This article describes the development of latent epoxy resins, the fabrication of test articles, and the mechanical properties measured from experimental joints compared with conventional, co-cured laminates. Methods of in-line quality control using and infrared spectroscopy and post-assembly forensics are also described. The final mode-II fracture toughness measured from precracked AERoBOND specimens was similar to that measured from co-cured laminates indicating that later cure epoxy materials could be a suitable replacement for secondary bonding.

Polymer-matrix composites (PMCs)↗
NASA NTRS1975

Effect of post cure time and temperature on the properties of two phenolic-fiber composites

Some effects of post-cure time and temperature on the physicomechanical properties of a phenolic-asbestos and a phenolic-glass composite are studied. The molding and post-curing procedures are discussed along with physical and mechanical test results. It is found that the specific gravity of the panels tested decreased slightly but the hardness always increased with post cure, and that the mechanical properties had different patterns of response to increasing post-cure time and temperature. For tensile properties, strength decreased, modulus increased, and elongation at break exhibited little change. In general, the phenolic-asbestos showed more positive response to post cure than did the phenolic-glass. Mold venting is found to impart better properties to the composites concerned.

Lucy, M. H.↗