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NASA NTRS2013

Process Optimization of Bismaleimide (BMI) Resin Infused Carbon Fiber Composite

Engineers today are presented with the opportunity to design and build the next generation of space vehicles out of the lightest, strongest, and most durable materials available. Composites offer excellent structural characteristics and outstanding reliability in many forms that will be utilized in future aerospace applications including the Commercial Crew and Cargo Program and the Orion space capsule. NASA's Composites for Exploration (CoEx) project researches the various methods of manufacturing composite materials of different fiber characteristics while using proven infusion methods of different resin compositions. Development and testing on these different material combinations will provide engineers the opportunity to produce optimal material compounds for multidisciplinary applications. Through the CoEx project, engineers pursue the opportunity to research and develop repair patch procedures for damaged spacecraft. Working in conjunction with Raptor Resins Inc., NASA engineers are utilizing high flow liquid infusion molding practices to manufacture high-temperature composite parts comprised of intermediate modulus 7 (IM7) carbon fiber material. IM7 is a continuous, high-tensile strength composite with outstanding structural qualities such as high shear strength, tensile strength and modulus as well as excellent corrosion, creep, and fatigue resistance. IM7 carbon fiber, combined with existing thermoset and thermoplastic resin systems, can provide improvements in material strength reinforcement and deformation-resistant properties for high-temperature applications. Void analysis of the different layups of the IM7 material discovered the largest total void composition within the [ +45 , 90 , 90 , -45 ] composite panel. Tensile and compressional testing proved the highest mechanical strength was found in the [0 4] layup. This paper further investigates the infusion procedure of a low-cost/high-performance BMI resin into an IM7 carbon fiber material and the optical, chemical, and mechanical analyses performed.

Ehrlich, Joshua W.↗

NASA NTRS2013

Experimental and Analytical Characterization of the Macromechanical Response for Triaxial Braided Composite Materials

Increasingly, carbon composite structures are being used in aerospace applications. Their highstrength, high-stiffness, and low-weight properties make them good candidates for replacing many aerospace structures currently made of aluminum or steel. Recently, many of the aircraft engine manufacturers have developed new commercial jet engines that will use composite fan cases. Instead of using traditional composite layup techniques, these new fan cases will use a triaxially braided pattern, which improves case performance. The impact characteristics of composite materials for jet engine fan case applications have been an important research topic because Federal regulations require that an engine case be able to contain a blade and blade fragments during an engine blade-out event. Once the impact characteristics of these triaxial braided materials become known, computer models can be developed to simulate a jet engine blade-out event, thus reducing cost and time in the development of these composite jet engine cases. The two main problems that have arisen in this area of research are that the properties for these materials have not been fully determined and computationally efficient computer models, which incorporate much of the microscale deformation and failure mechanisms, are not available. The research reported herein addresses some of the deficiencies present in previous research regarding these triaxial braided composite materials. The current research develops new techniques to accurately quantify the material properties of the triaxial braided composite materials. New test methods are developed for the polymer resin composite constituent and representative composite coupons. These methods expand previous research by using novel specimen designs along with using a noncontact measuring system that is also capable of identifying and quantifying many of the microscale failure mechanisms present in the materials. Finally, using the data gathered, a new hybrid micromacromechanical computer model is created to simulate the behavior of these composite material systems under static and ballistic impact loading using the test data acquired. The model also quantifies the way in which the fiber/matrix interface affects material response under static and impact loading. The results show that the test methods are capable of accurately quantifying the polymer resin under a variety of strain rates and temperature for three loading conditions. The resin strength and stiffness data show a clear rate and temperature dependence. The data also show the hydrostatic stress effects and hysteresis, all of which can be used by researchers developing composite constitutive models for the resins. The results for the composite data reveal noticeable differences in strength, failure strain, and stiffness in the different material systems presented. The investigations into the microscale failure mechanisms provide information about the nature of the different material system behaviors. Finally, the developed computer model predicts composite static strength and stiffness to within 10 percent of the gathered test data and also agrees with composite impact data, where available.

Littell, Justin D.↗

NASA NTRS1993

Analysis of pultrusion processing for long fiber reinforced thermoplastic composite system

Pultrusion is one of the composite processing technology, commonly recognized as a simple and cost-effective means for the manufacturing of fiber-reinforced, resin matrix composite parts with different regular geometries. Previously, because the majority of the pultruded composite parts were made of thermosetting resin matrix, emphasis of the analysis on the process has been on the conservation of energy from various sources, such as heat conduction and the curing kinetics of the resin system. Analysis on the flow aspect of the process was almost absent in the literature for thermosetting process. With the increasing uses of thermoplastic materials, it is desirable to obtain the detailed velocity and pressure profiles inside the pultrusion die. Using a modified Darcy's law for flow through porous media, closed form analytical solutions for the velocity and pressure distributions inside the pultrusion die are obtained for the first time. This enables us to estimate the magnitude of viscous dissipation and it's effects on the pultruded parts. Pulling forces refined in the pultrusion processing are also analyzed. The analytical model derived in this study can be used to advance our knowledge and control of the pultrusion process for fiber reinforced thermoplastic composite parts.

Tso, W.↗

DOE OSTI2023

Subcomponent Validation of Composite Joints for the Marine Energy Advanced Materials Project

The Marine Energy Advanced Materials project is an ongoing multi-year, multi-lab project with the main goals of addressing barriers and uncertainties facing marine energy developers in adopting advanced materials for structural applications. NREL's goals of the project were to address subcomponents testing needs for marine energy materials, to improve understanding of design allowables at the full-scale and provide near net-scale static and fatigue data of composite subcomponents using materials applicable to the marine energy industry. In the long term, the test method development and data generated would be used to inform standards development. This report outlines perhaps one of the largest-scale studies conducted with regards to saltwater conditioning of various composite material subcomponents and their subsequent structural validation, specifically directed at the marine renewable energy industry. A variety of fiberglass composite panels with epoxy and vinyl ester epoxy resin systems were manufactured at Montana State University, which were then used to manufacture an array of different types of subcomponent test specimens at the National Renewable Energy Laboratory's Flatirons Campus. These subcomponents were in the form of T-bolt and double-ended-insert specimens, which were intended to represent bonded and mechanical bolted connections for thick composite laminates, metal-metal and composite lap shear specimens to evaluate adhesion of constituent materials, and adhesive beam-shear specimens as part of an effort to better evaluate the characteristics of thick adhesive bondlines. Overall, the materials used were fiberglass reinforced epoxy and vinyl ester matrix composites, epoxy and methacrylate adhesives, and 316 and 2507 stainless steels. Specimens were then conditioned in salt water at various temperatures and for various periods of time at Florida Atlantic University and Pacific Northwest National Laboratory. All specimens were then mechanically characterized and validated using various test methods under static and fatigue loading conditions at NREL's Structural Technology Laboratory. Throughout the conditioning and mechanical validation process, valuable experience was gained, which will help guide future test method development for marine energy materials. In many instances, the results indicated similar observations as to what had been observed during previous coupon scale characterization efforts that provided a vital understanding of the scale up process. However in some instances, unexpected phenomena were observed, such as interactions between the adhesives and 316 steel. Furthermore, some materials exhibited significant degradation due to the saltwater conditioning. Ultimately, this report provides a detailed summary of the specimens that were designed, the subcomponent test methods that were developed, and the results that were generated, which will serve as important guidance for marine renewable energy developers and researchers for future structural designs and validation.

16 TIDAL AND WAVE POWER↗

NASA NTRS1984

Electron radiation effects on the thermal expansion of graphite/resin composites

The effects of 1 MeV electron radiation on the thermal expansion characteristics of two graphite reinforced resin matrix composite systems were studied. Specimens of both graphite/epoxy (T300/5208) and graphite/polyimide (C6000/PMR15) were irradiated to a total dose of 6 x 10 to the 9th rads at two different rates. Dynamic mechanical analyses (DMA) were performed to study changes in resin chemistry. Thermal expansion results indicate that radiation did produce permanent residual strains of up to -70 x 10 to the -6th for the graphite/epoxy when exposed to temperatures up to +280 F. However, no permaanent changes in the coefficient of thermal expansion (CTE) were observed. No permanent residual strains or changes in the CTE attributable to radiation were observed for the graphite/polyimide specimens. DMA results indicate that electron radiation caused chemical changes in the epoxy matrix. These changes resulted in a lower glass transition temperature and broader 'rubbery region' which extended into the temperature range of the thermal expansion tests.

Bowles, D. E.↗

NASA NTRS1981

Development of orthotropic birefringent materials for photoelastic stress analysis

Materials were selected and fabrication procedures developed for orthotropic birefringent materials. An epoxy resin (Maraset 658/558 system) was selected as the matrix material. Fibers obtained from style 3733 glass cloth and type 1062 glass roving were used as reinforcement. Two different fabrication procedures were used. In the first one, layers of unidirectional fibers removed from the glass cloth were stacked, impregnated with resin, bagged and cured in the autoclave at an elevated temperature. In the second procedure, the glass roving was drywound over metal frames, impregnated with resin and cured at room temperature under pressure and vacuum in an autoclave. Unidirectional, angle-ply and quasi-isotropic laminates of two thicknesses and with embedded flaws were fabricated. The matrix and the unidirectional glass/epoxy material were fully characterized. The density, fiber volume ratio, mechanical, and optical properties were determined. The fiber volume ratio was over 0.50. Birefringent properties were in good agreement with predictions based on a stress proportioning concept and also, with one exception, with properties predicted by a finite element analysis.

Daniel, I. M.↗

NASA NTRS1984

Development and characterization of orthotropic-birefringent materials

Daniel, I. M.↗

NASA NTRS1985

Differences in interfacial bond strengths of graphite fiber-epoxy resin composites

The effect of epoxy-size and degree of cure on the interfacial bonding of an epoxy-amine-graphite fiber composite system is examined. The role of the fiber-resin interface in determining the overall mechanical properties of composites is poorly understood. A good interfacial adhesive bond is required to achieve maximum stress transfer to the fibers in composites, but at the same time some form of energy absorbing interfacial interaction is needed to achieve high fracture toughening. The incompatibility of these two processes makes it important to understand the nature and basic factors involved at the fiber-resin interface as stress is applied. The mechanical properties including interlaminar shear values for graphite fiber-resin composites are low compared to glass and boron-resin composites. These differences have been attributed to poor fiber-matrix adhesion. Graphite fibers are commonly subjected to post-treatments including application of organic sizing in order to improve their compatibility with the resin matrix and to protect the fiber tow from damage during processing and lay-up. In such processes, sized graphite fiber tow is impregnated with epoxy resin and then layed-up i nto the appropriate configuration. Following an extended ambient temperature cure, the graphite-resin composite structure is cured at elevated temperature using a programmed temperature sequence to cure and then cool the product.

Needles, H. L.↗

NASA NTRS1984

Fundamental Studies of Composite Toughness

Evaluation of drop weight impact testing of neat resin and crossplied graphite fiber reinforced composites resulted in three conclusions: (1) during impact of cross-ply laminates, resin properties appear to influence the extent and mechanism of damage propagation; (2) by itself, neat resin strain to fracture is not a controlling influence on resin or composite fracture toughness; and (3) impact failure energy of neat resin plates can give a misleading indication of the resin contribution to composite impact behavior because of differences in the magnitude of diaphragm action in the two systems. Both geometric and composite constituent materials properties influence the drop weight impact resistance of crossplied composite plates. The matrix influence appears to be reflected in the incipient damage mechanism and the propagation of damage.

Bowles, K. J.↗

NASA NTRS1974

Resin/graphite fiber composites

Techniques were developed that provided thermo-oxidatively stable A-type polyimide/graphite fiber composites using the approach of in situ polymerization of monomeric reactants directly on reinforcing fibers, rather than employing separately prepared prepolymer varnish. This was accomplished by simply mixing methylene dianiline and two ester-acids and applying this solution to the fibers for subsequent molding. Five different formulated molecular weight resins were examined, and an optimized die molding procedure established for the 1500 formulated molecular weight system. Extensive ultrasonic inspection of composites was successfully utilized as a technique for monitoring laminate quality. Composite mechanical property studies were conducted with this polyimide resin at room temperature and after various time exposures in a thermo-oxidative environment at 561 K (550 F), 589 K (600 F) and 617 K (650 F). It was determined that such composites have a long term life in the temperature range of 561 K to 589 K. The final phase involved the fabrication and evaluation of a series of demonstration airfoil specimens.

Cavano, P. J.↗

DOE OSTI2021

Extraction of radium and actinium with Pb resin and Rose Bengal

The extraction of radium and actinium with Eichrom Pb resin and Rose Bengal has been studied. Radium and actinium both show a strong affinity (k’ > 10,000) for the resin at intermediate pHs (~ 5–7) from solutions with Rose Bengal. The pH range and magnitude of uptake for both radium and actinium is significantly increased by the presence of Rose Bengal compared to basic solutions without this counter ion. Additionally, radium uptake is extremely fast from basic solutions with and without Rose Bengal; actinium uptake is slower, particularly in solutions without Rose Bengal. Column studies show that despite the similar behavior of actinium and radium in this system, separations of these two elements with Pb resin and Rose Bengal solutions are possible with reasonable yields due to the differences in uptake kinetics.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2022

Characterization of the Emissions and Crystalline Silica Content of Airborne Dust Generated from Grinding Natural and Engineered Stones

Abstract In this study, we systematically characterized the airborne dust generated from grinding engineered and natural stone products using a laboratory testing system designed and operated to collect representative respirable dust samples. Four stone samples tested included two engineered stones consisting of crystalline silica in a polyester resin matrix (formulations differed with Stones A having up to 90wt% crystalline silica and Stone B up to 50wt% crystalline silica), an engineered stone consisting of recycled glass in a cement matrix (Stone C), and a granite. Aerosol samples were collected by respirable dust samplers, total dust samplers, and a Micro-Orifice Uniform Deposit Impactor. Aerosol samples were analyzed by gravimetric analysis and x-ray diffraction to determine dust generation rates, crystalline silica generation rates, and crystalline silica content. Additionally, bulk dust settled on the floor of the testing system was analyzed for crystalline silica content. Real-time particle size distributions were measured using an Aerodynamic Particle Sizer. All stone types generated similar trimodal lognormal number-weighted particle size distributions during grinding with the most prominent mode at an aerodynamic diameter of about 2.0-2.3 μm, suggesting dust formation from grinding different stones is similar. Bulk dust from Stone C contained no crystalline silica. Bulk dust from Stone A, Stone B, and granite contained 60, 23, and 30wt% crystalline silica, respectively. In Stones A and B, the cristobalite form of crystalline silica was more plentiful than the quartz form. Only the quartz form was detected in granite. The bulk dust, respirable dust, and total dust for each stone had comparable amounts of crystalline silica, suggesting that crystalline silica content in the bulk dust could be representative of that in respirable dust generated during grinding. Granite generated more dust per unit volume of material removed than the engineered stones, which all had similar normalized dust generation rates. Stone A had the highest normalized generation rates of crystalline silica, followed by granite, Stone B, and Stone C (no crystalline silica), which likely leads to the same trend of respirable crystalline silica (RCS) exposure when working with these different stones. Manufacturing and adoption of engineered stone products with formulations such as Stone B or Stone C could potentially lower or eliminate RCS exposure risks. Combining all the effects of dust generation rate, size-dependent silica content, and respirable fraction, the highest normalized generation rate of RCS consistently occurs at 3.2-5.6 µm for all the stones containing crystalline silica. Therefore, removing particles in this size range near the generation sources should be prioritized when developing engineering control measures.

Public, Environmental & Occupational Health↗

NASA NTRS1986

The effect of resin toughness and modulus on compressive failure modes of quasi-isotropic graphite/epoxy laminates

Compressive failure mechanisms in quasi-isotropic graphite/epoxy laminates were characterized for both unnotched and notched specimens and also following damage by impact. Two types of fibers (Thornel 300 and 700) and four resin systems (Narmco 5208, American Cyanamid BP907, and Union Carbide 4901/MDA and 4901/mPDA) were studied. For all material combinations, failure of unnotched specimens was initiated by kinking of fibers in the 0-degree plies. A major difference was observed, however, in the mode of failure propagation after the 0-degree ply failure. The strength of quasi-isotropic laminates in general increased with increasing resin tensile modulus. The laminates made with Thornel 700 fibers exhibited slightly lower compressive strengths than did the laminates made with Thornel 300 fibers. The notch sensitivity as measured by the hole strength was lowest for the BP907 resin and highest for the 5208 resin. For the materials studied, however, the type of fiber had no effect on the notch sensitivity.

Sohi, M. M.↗

NASA NTRS1987

The effect of resin toughness and modulus on compressive failure modes of quasi-isotropic graphite/epoxy laminates

Hahn, H. Thomas↗

DOE OSTI2023

Large-scale computational polymer solubility predictions and applications to dissolution-based plastic recycling

Dissolution-based plastic recycling is a promising approach to separate and recover high quality pure polymer resins from multicomponent plastic waste by exploiting differences in polymer solubility. The design of a dissolution-based polymer recycling process requires the selection of appropriate solvent systems and operating temperatures to dissolve only target polymers. Determining these parameters experimentally is challenging due to the wide range of solvents and temperatures possible for a given set of target polymers. In this work, we report a computational scheme that employs molecular dynamics simulations and the Conductor-like Screening Model for Realistic Solvents to predict polymer solubilities. Using this scheme, we established a computational solubility database for 8 common polymers and 1007 solvents at multiple temperatures and measured selected solubilities experimentally to validate computational predictions. Analysis of functional groups within this large database then provides chemical heuristics relating the molecular structures of good and non-solvents for selected polymers. We further developed a tool that automates the selection of solvents for all possible sequences in which target polymers can be selectively dissolved to guide the design of dissolution-based plastic recycling processes. Here, we demonstrate the application of these methods via multiple experimental case studies of representative dissolution-based polymer recycling processes in which pure polymer resins were successfully recovered from physical mixtures of polymers.

42 ENGINEERING↗

NASA NTRS1993

Development of RTM and powder prepreg resins for subsonic aircraft primary structures

Dow developed a thermoset resin which could be used to produce composites via the RTM process. The composites formed are useful at 200 F service temperatures after moisture saturation, and are tough systems that are suitable for subsonic aircraft primary structure. At NASA's request, Dow also developed a modified version of the RTM resin system which was suitable for use in producing powder prepreg. In the course of developing the RTM and powder versions of these resins, over 50 different new materials were produced and evaluated.

Woo, Edmund P.↗

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↗

DOE OSTI2024

Cast Film Production with Polyethylene Recycled from a Post-Industrial Printed Multilayer Film by Solvent-Targeted Recovery and Precipitation

The solvent-targeted recovery and precipitation (STRAP) process separates and recovers the constituent resins in multilayer plastic packaging films by selective polymer dissolution. In this work, three different experimental methods were considered to recover a polyethylene (PE) resin from a printed multilayer film by STRAP. The methods consisted of (1) a filter bag system, (2) a Soxhlet extraction, and (3) a jacketed dissolution vessel. Cast films were produced with the PE recovered from each method and were analyzed for color, mechanical properties, and number of impurities. High-quality recycled PE cast films can be produced by increasing the solvent to plastic ratio, including a filter pore size of 100 μm, and optimizing temperature control in STRAP. Furthermore, this study demonstrates that STRAP polymers can be recycled back into plastic films, enabling the potential circularity of these packaging materials.

36 MATERIALS SCIENCE↗