Continuous Fiber 3D printing for Compression Over Molding
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The ongoing pursuit of improved fuel economy and reduced greenhouse gas emissions has resulted in sustained interest for lightweight materials technologies. In this context, carbon fiber composites have captured the imagination of automotive engineers due to the potential to achieve substantial mass reduction when compared to traditional steel construction. That stated, the use of carbon fiber composites in automotive has been limited for the most part to premium supercars and other derivative platforms. In these cases, manufacturing costs are less of an obstacle to implementation, and the performance benefits of carbon fiber have enabled production of structures offering more than 50% weight savings. In practice, translating these low-volume demonstrations onto high-volume vehicle platforms has remained challenging. This can be attributed to several factors, with the absence of suitable high throughput production methodologies being a key impediment. To date, structural, crash critical components have relied upon manufacturing techniques born out of the aerospace industry. This has created a disconnect between automotive production systems that are accustomed to manufacturing multiple parts per minute and the aerospace technologies that have cycle times in the order of hours. Consequently, the focus of this project is the development of manufacturing process technology for carbon fiber composites that can support a mainstream vehicle program at an assumed throughput of 100,000 vehicles per year. In practice, this translates to a part-to-part cycle time of less than 3 minutes. Project participation included contributions from a broad range of academic, industrial and national lab partners. The primary scope of work, being the development of new carbon fiber epoxy compounds that are stable at room temperature and suited to high throughput automated processing. For project management, the work streams were divided into six key areas, with the lead organization in parentheses. • Carbon fiber/epoxy materials formulation development and scale up (Dow) • Simulation of discontinuous near isotropic meso-structure intermediates (Purdue) • Simulation of mechanical performance of compression molded components (Purdue) • Meso-Scale morphological analysis and correlation with structural performance (UTK) • Paint and adhesion durability analysis (MSU) • Demonstrator part design, prototype production, and validation testing (Ford). The primary goal at the commencement of the project was development of a chopped carbon fiber sheet molding compound (SMC) that offered a three times improvement in tensile modulus over a comparable glass-based SMC. In addition to meeting mechanical performance targets, the resin kinetics were modified to achieve a processing cycle time of less than 3 minutes. Other critical-to-quality (CTQ) specifications were also stipulated to account for a broad range of materials and processing characteristics. To achieve the above, staff scientists at Dow Chemical created an extensive series of new epoxy blends for testing and validation. Throughout this development, a key challenge was attaining material performance goals without impacting processing behavior and paintability of finished components. The latter required a new internal mold release system being developed by Dow that was designed to complement the kinetics of the rapid cure epoxy. As a complement to work studies at the industrial partners, the teams from academia executed a series of analytical and experimental studies to investigate potential factors influencing CF-SMC performance. Unit cell models were developed to capture the meso-scale representations of the fiber matrix architecture. Results of this analysis and subsequent morphological investigations led to the design of a novel composite derivative comprising carbon fiber platelets embedded in an epoxy matrix; the platelet size and aspect ratio playing significant role in final composite properties. This approach was a departure from previous research in CF-SMC development whereby bulk filamentization or disassembly of the carbon fiber rovings had been considered the most effective means of achieving both fiber wet through and wet-out. As the course of the academia studies progressed, the aspect ratio of the fiber constituents was further optimized before finalizing material attributes and processing conditions. For the purposes of technology validation, the Ford team led a work stream devoted to the design, fabrication and testing of demonstration components. The carbon fiber SMC material has the potential to displace numerous stampings and castings on an automotive structure but ultimately vehicle closure applications were selected to showcase the abilities of the CF-SMC to achieve both mass reduction and business case for large complex structures. Using target properties established by the Dow staff scientists, the complete closure system for a full-size sedan decklid and a mid-size wagon liftgate were engineered. Prototypes for both applications were fabricated using production representative processing methods to allow for physical testing and performance validation of the CF-SMC structures. Following completion of a testing program that concluded with a FMVSS301 55 mph offset rear crash, the CF-SMC formulation was declared by the Ford team to have met all engineering requirements. To summarize, the joint development activities during this project led to significant technical breakthroughs and achievement of all milestones. The result was the development of a novel, tack-free carbon fiber molding compound that is suited to automated processing. This combined room temperature stability, fast cure kinetics, and internal mold release system facilitates cycle times that are conducive to high-volume production. The VORAFUSE M6400 successfully passed technology validation at Ford and is now eligible for consideration on future production commercial vehicle programs.
With the growing demand for enhanced automotive fuel efficiency and environmental sustainability, there is a need for lightweighting automotive components through innovative design and manufacturing processes. Here, this study leverages a combination of numerical iterative design optimization and hybrid additive manufacturing–compression molding (AM-CM) technique for metal polymer composites to lightweight an automotive seatback. The AM-CM process enables robust mechanical interlocking between metals and composites, boasting high stiffness and strength with low overall density. Replacing metallic components with such metal polymer composites allows for comparable mechanical performance while significantly reducing the overall weight. First, the automotive seatback design space is reduced to critical load carrying regions using topology optimization and high stress concentration areas are identified using finite element analysis. Next, a lightweight metal polymer subcomponent is designed for a high stress concentration region. The full seatback frame with spatially heterogeneous material-specific design is then iteratively optimized to enable enhanced stiffness with minimal weight. Overall, the automotive seatback frame designed with location-specific metal, polymer, and metal polymer composite materials weighs 20% less than the metal-only design while exhibiting similar stiffness.
The purpose of this project task was to make automotive composite part manufacturing more cost competitive for low volume production and thereby drive composite application innovation. The strategy was to incorporate low-cost preforming, snap cure resins, and RapidClave® processing to create an alternative to conventional automotive composite manufacturing based on SMC. The program used RapidClave® technology from Globe Machine Manufacturing, fast-curing (“snap cure”) epoxy resins from Hexion, and conformable/stretchable glass fiber reinforcement mats produced by Owens Corning for rapid preforming. O’Gara Armoring retrofits vehicles to meet special security needs, such as larger doors to facilitate easier entry into the vehicle. O’Gara has a variety of custom vehicles in need of custom doors that require affordable tooling to produce approximately 100 ship sets/year. The project focused on a composite door panel application provided by O’Gara that is currently made by manual chopped fiber spray-up processing. UDRI reverse-engineered the current composite door panel and created tooling for use in the RapidClave®. UDRI designed an improved composite door using MultiMat fiberglass reinforcement from Owens Corning. UDRI made snap cure resin films from Hexion resin. Finally, UDRI conducted molding trials to compare autoclave processing with RapidClave® processing. The technical goals of the project were to reduce tooling cost by 50% as compared to SMC compression molding and to reduce cycle time by 50% compared to current manual spray-up process. The approach to reduce tool costs is based on use of single sided tooling for use at 100 psi, as compared to matched metal SMC tooling. An added benefit realized from the program is that the Owens Corning mat provided more uniform thickness and improved performance. Tensile and flexural strengths and moduli were increased by at least 50%. This task also demonstrated a 75% decrease in cycle time. O’Gara is evaluating the technology demonstrated in this project for some of their current production. Additionally, there are new products O’Gara is pursuing which require higher production rates than their current products. O’Gara has identified these new products as good candidates for the RapidClave® technology. The cost advantages demonstrated by this project would then lead to significant economic development. In conclusion, this task successfully combined the RapidClave® technology from Globe with a snap cure epoxy resin film system from Hexion and preform material from Owens Corning. Further research is needed to better map the technical limits such as cycle time of these technologies. Additionally, the technology should be extended in terms of size and shape to include large parts outside of automotive applications, such as a small aircraft fuselage.
Oak Ridge National Laboratory (ORNL) worked with DowAksa Industry to investigate the potential of using PA66 material to produce larger composite parts, transcending the limitations of traditional presses. The project aimed to develop a suitable material for printing battery boxes using Nylon 66 infused with 40 wt.% carbon fiber, compatible with the ORNL Additive Manufacturing and Compression Molding (AM-CM) system. However, even with extensive work, it was concluded that the material is not compatible with the AMCM process and suitable for joining using compression technique. Main reason for the incompatibility were found to be very high crystallinity of the PA66 grade chosen for this work. To improve printability, a modifier (proprietary) was added to decrease crystallinity, but this led to reduced thermal stability and adhesion issues.
Permanent magnets are expected to play a crucial role in the realization of the clean economy. In particular, the neodymium-iron-boron (Nd2Fe14B or NdFeB) magnets, which have the highest energy density among rare earth permanent magnets, are needed for building more efficient windmill generators, electric vehicle motors, etc. Currently, near-net shape magnets can be either made through sintering and compression molding with extensive post machining or directly through injection molding. However, injection molding has a loading volume fraction limitation of 0.65 for nylon binders. A novel method of manufacturing bonded permanent magnets with loading fraction greater than 0.65 has been demonstrated using Big Area Additive Manufacturing (BAAM) printers. As energy density is directly proportional to the square of the magnet loading fraction, magnets produced using BAAM printers require less volume and magnetic material compared to that of injection molded magnets on average. A comparative LCA shows that this difference in magnetic powder consumption nearly constitutes the difference in the environmental impact categories. Even after assuming recycled magnetic input, the BAAM magnets perform better environmentally than injection molded magnets, especially in the ozone depletion category. Since BAAM printers can accommodate even higher loading fractions, at scale, BAAM printers possibly can bring about a significant decrease in rare earth mineral consumption and environmental emissions. So furthermore, single screw extrusion enables BAAM printers to have high print speeds and allow them to be economically competitive against injection molding. Therefore, BAAM printed magnets show promise in transitioning towards the clean economy.
The global composite industry generates large quantities of waste and which mostly end as landfill due to lack of meaningful end-use applications for the multiple waste streams. In a recent report by the Electric Power Research Institute (EPRI), waste generated by the wind industry could reach 370,000 tons a year of composite wind energy blades being decommissioned and scrapped. Wind energy is just one major industry utilizing composite materials. The waste generated by industry includes End-of-Life (EoL) materials and manufacturing process scrap. GreenTex Solutions has developed a unique and innovative technology to recycle the composite waste streams in a range of forms made from production waste and EoL materials. This includes manufacturing waste materials such as dry chopped fiber tow, loose fibers, shredded fibers from reinforcement fabrics, cured/semi-cured prepregs, and it also includes fully-cured composite structure waste (such as edge trims from cured parts) from manufacturing aircraft, automobiles, wind blades, boats, and composite cylinders (tanks). Current recycling methods involve recovering the structural fiber by removing the matrix resin through methods such as pyrolysis. The resulting fibers are used in injection molding or wet laid nonwoven mats and other usable forms. The GreenTex technology bypasses these intermediate steps to create the lowest possible recycling processing costs and the lowest embodied energy/CO2 emissions. The end-product from the GreenTex technology is a finished industrial composite part/application versus intermediate fibers or fabrics. The GreenTex manufacturing process enables cross-industry reuse of recycled feedstock by taking waste from multiple industries (wind energy, aerospace, marine, etc.) and recycles the waste into a product used in other industries. The initial target market application is structural flooring for intermodal shipping containers and truck bodies. One of the team’s key partners is Wabash National which produced 29,000 truck bodies in 2019. The current flooring system is comprised of solid oak “butcher board” laminated panels. Additionally, Mediterranean Shipping Containers (MSC) transports over 1.8 million twenty-foot equivalent units per year in intermodal shipping containers. The current container floor is laminated hardwood that is harvested from the rain forests of Central and South America. The project is to develop a flooring system made from recycled composites that can be qualified for both companies (Wabash and MSC). Initial prototypes validated that the recycled composites panels are lighter and thinner with much higher mechanical strength. These results suggest a typical truck trailer would have 20% lower tare weight. The GreenTex technology is not limited to flooring and is widely applicable to other transportation elements such as walls, roof elements, cab areas and related structural components. Under this project different composite waste streams were evaluated and then combined to develop a formulation that would meet the targeted performance criteria for a flooring system. Wet compression molding was used to fabricate plaques at different tonnage using various composite waste streams. The plaques were tested for flexure and impact.
Traditionally, thermoset resins such as polyesters (PE) and epoxies are used as the polymer matrix for construction of wind turbine blades. However, concern about their end-of-life treatment garners interest to use thermoplastics for increased recyclability. However, the high viscosity of molten thermoplastics inhibits their use in manufacturing wind turbine blades with injection or compression molding. A recently developed, infusible, reactive thermoplastic resin overcomes this technological barrier. Toward verifying that this recyclable resin is suitable for use in wind turbine blades, a dataset of R?=?0.1 and R?=?10 fatigue data for glass fiber-reinforced acrylic composites is provided and equal fatigue life to industry standard epoxy and unsaturated PE resin systems is demonstrated. Specifically, R?=?0.1 fatigue data for acrylic composites at room temperature and -30?degrees C for verification of low-temperature performance are tabulated. To elucidate failure mechanisms, in situ mechanical testing with X-ray computed tomography demonstrates that damage accumulation occurs by crack propagation along the fiber-matrix interface under cyclic loading. Infrared (IR) thermography predicts failure points in composites specimens with porosity defects introduced from nonideal manufacturing processes. Furthermore, these manufacturing defects are shown to compromise the fatigue life of the acrylic laminates by an order of magnitude.
Controlling fiber orientation and porosity in short-fiber thermoplastic composites is important for enhancing mechanical, electrical and thermal properties in large-format additive manufacturing. This study employs a factorial design of experiments (DoE) to assess the effects of nozzle diameter (5.08 mm–10.16 mm), temperature (230–250 °C), and extruder screw speed (150–280 rpm) on flow rate, shear rate, porosity, fiber orientation, fiber length and tensile strength in 20 % carbon fiber-filled acrylonitrile butadiene styrene. ANOVA results show that screw speed significantly impacts flow rate, while nozzle diameter and temperature have lesser effects. Shear rate increases with smaller nozzles and higher speeds. Porosity decreases from 5.58 % with a 10.16 mm nozzle to 3.11 % with a 5.08 mm nozzle at 150 rpm due to increased shear rates, which induce shear thinning, reducing viscosity and facilitating gas escape. Larger nozzles (10.16 mm) produce larger, more heterogeneous pores, while smaller nozzles (5.08 mm) yield smaller, uniform pores. Beads produced with the 5.08 mm nozzle exhibit longer fiber lengths due to reduced residence time, lower shear stress, and better alignment. Fiber orientation improves with smaller nozzles due to higher shear rates but decreases with higher screw speeds (280 rpm) due to shorter residence times. The highest fiber alignment (A xx ∼ 0.65) and low porosity (∼3%) were achieved with a 5.08 mm nozzle at 150 rpm, while equivalent additive manufacturing-compression molding samples exhibited better tensile strength (∼93 MPa) under these conditions. In conclusion, these findings emphasize the importance of optimizing processing parameters to enhance fiber alignment and reduce porosity for improved mechanical performance.
Compatibility between the reinforcing phase and the polymer matrix is critical to achieving the desired mechanical and thermal performance of composite materials. Several mechanisms can enhance this interfacial interaction, including surface treatments (e.g., oxidation, plasma, or irradiation), in-situ nanoparticle deposition, and fiber sizing. Here, in this study, cellulose nanofibrils (CNF) were employed as a sustainable sizing agent to modify the interface in commingled carbon fiber (CF)/polyamide 6 (PA 6) yarns, in which CF and PA6 filaments are intimately blended to enable simultaneous consolidation. A 0.25 wt% CNF aqueous suspension was applied under bath sonication to ensure uniform dispersion and minimize agglomeration. CNF-sized and unsized yarns were used to fabricate unidirectional composite plates via filament winding on a flat mandrel, followed by compression molding. Scanning electron microscopy confirmed CNF presence on both CF and PA6 filaments. CNF-sized composites exhibited increments in interlaminar shear strength (ILSS) by 50%, flexural strength by 11%, and tensile strength by 2.5% compared to unsized composites. Thermal analysis showed minimal changes in degradation temperature and crystallinity. These findings demonstrate that CNF sizing enhances interfacial bonding and mechanical performance, offering a scalable and environmentally friendly strategy for thermoplastic composite manufacturing along with yarn/tow handleability.
Fused deposition modeling (FDM) printed polymers are rarely used as a structural material due to anisotropic and low mechanical properties compared with conventional composites. In recent years, greater need has been expressed for recycling of materials, such as recyclable FDM, at the end of service life to reduce environmental pollution and manufacture cost. However, how the amount of resin uptake in the skin and skin/core interphase affects the bending and shear performance of the sandwich composites when replacing the low strength and ductile core (conventional core) with a high strength and brittle core (FDM printed PLA (polylactic acid) core) still remains unclear. A new manufacturing routine is needed to improve the incorporation of FDM printed polymers in composite structures. In this work, FDM printed PLA was used as core material and sandwiched between two unidirectional glass fiber reinforced polymer (GFRP) skins to form a sandwich composite by compression-molding (CM) process, which provides a good manufacturing strategy for skin/core interphase modification. The significance of the CM process is proved by investigating the effect of resin uptake on bending and in-plane/out-of-plane shear performances. Current first order shear deformation (FSDT) theory lacks a direct connection between the in-plane shear stress and out-of-shear stress in the core region of sandwich composites. With the help of DIC, a connection between the in-plane shear and the out-of-plane shear strain was built and in-plane shear properties can acquire through out-of-plane shear properties, hence reducing the redundancy of sample preparation or the need for simulation. A significant improvement was found compared with the optimized resin uptake (Optimized resin uptake range: 20.43%–22.86 wt%) 3D-printed PLA core sandwich composite and lowest performance sandwich composite (Improvement: in-plane shear strength (~34%)/modulus (~29%), out-of-plane shear strength (~25%)/modulus (~31%), specific peak bending load (~19%)). Finally, compared with balsa core sandwich composites, the 3D-printed cores are suitable for use in composite sandwich structures in many applications with a satisfactory strength-to-weight ratio.
The end-of-life vehicles (ELV) regulations motivate hybrid materials usage in automotive industries to optimize properties at reduced cost and increase eco-friendly designs. This research explores hybrid compositions of natural bamboo fiber and synthetic carbon fiber. The goal of hybridization was to synergistically benefit from each constituent– i.e., sustainability, energy absorption and superior damping from bamboo, and high strength and stiffness from carbon fiber. Carbon fibers (CF), bamboo fibers (BF) and polypropylene (PP) fibers were dispersed in water to produce wet-laid hybrid mats. The mats were compression molded into consolidated panels to obtain the hybrid composite(s) (BF-CF-PP). Four formulations with different fiber-resin weight percent were designed and produced including- BF-PP (30/70), BF-PP (50/50), BF-CF-PP (32/8/60), and BF-CF-PP (8/32/60). The effect of (a) fiber length, (b) surface treatment, (c) fiber content, and (d) consolidation pressure on the mechanical properties were examined. The improved mechanical (flexural strength 76.4 MPa, flexural modulus 4.1 GPa, ILSS 12.4 MPa and impact strength 49.9 KJ/m 2 ) and vibrational damping (1.05%) properties showed that the BF-CF-PP (8/32/60) provided higher properties compared to the other variants. The projected properties at various stoichiometric ratios of carbon and bamboo fiber revealed that the properties of hybrid composites could be tailored to produce desirable, cost-effective, and sustainable automotive components.
Natural fiber composites offer an advantage in terms of weight saving for many automotive applications; however, many natural fiber composites lack properties to justify substitution for synthetic composites. Hybridizing the natural fiber composites by adding a fraction of synthetic fibers is an innovative approach to provide a balance between composite's performance and weight savings. In this study, coir fiber (40 wt%)-reinforced polypropylene (PP) composites were hybridized by substituting a fraction of coir fiber with glass fiber (0–30 wt%). The composites were prepared using a novel wet-laid technique followed by compression molding, where the fiber length is preserved. The composites prepared by hybridizing PP/coir fibers with glass fibers were light in weight (6–20% lighter compared to 40 wt% glass fiber reinforced PP) with significantly enhanced tensile (strength – 49–182%, modulus – 54–130%), flexural (strength – 41–104%, modulus – 64–193%), and impact properties (157 - 474%) compared to 40 wt% coir fiber reinforced PP composites. Furthermore, the addition of glass fiber (10–30 wt%) to coir fiber reduced the water-absorbing tendency (by 18–74%) of PP/coir fiber composites. All in all, this work has potential applications in automotive, mass transit, and truck applications where natural fiber composites are being investigated as alternatives to metal and/or fully synthetic composites.
This work explores a type of composite called thermoplastic polymer-fiber-reinforced polymers (PFRPs), often referred to as self-reinforced composites (SRCs). A representative PFRP was exemplified using unidirectional (UD) ultra-high-molecular-weight polyethylene (UHMWPE) fibers embedded in a high-density polyethylene (HDPE) matrix. The effects of compression molding temperature and pressure on the mechanical and morphological behaviors of the filament-wound PFRPs with various fiber volume fractions (V f ) were experimentally investigated. The results elucidate the evolution of morphologies and tensile properties of the PFRPs due to thermal melting, fiber misalignment from pressure, and (V f )-induced structural variance, which has not been comprehensively reported yet. The highest specific tensile strength and modulus of the PFRP laminae reach 600 MPa/(g/cm 3 ) and 31 GPa/(g/cm 3 ), respectively. These properties are comparable to glass-/aramid-fiber-reinforced polymers (GFRPs, GFRTPs, AFRPs, and AFRTPs), with PFRPs exhibiting better ductility (specific strain at peak load ≈ 4%/(g/cm 3 )) than other common polymer composites. The motivation for this work was the high recyclability of PFRPs, which can be recycled by melting both the fibers and the matrix, and then reshaped them for re-manufacturing composites to maximize the efficiency in material reuse. This process simplifies the implementation of closed-loop recycling, re-manufacturing, and reuse to support sustainability in composites. This work aims to contribute to advancing thermoplastic PFRPs for their potential applications in various industries.
Composite manufacturing presents numerous challenges, as defects can arise from various sources throughout the process. In sandwich composite structures, the integration of a foam core introduces additional complexity and increases the likelihood of defect formation like delamination. To mitigate these issues and reduce the risk of future structural failures, in-situ monitoring during manufacturing is essential. This study investigates infrared (IR) thermography as a non-destructive technique for detecting manufacturing defects in foam-core sandwich composite panels under thermally excited conditions representative of in-situ processing. A stationary FLIR A8590 IR camera (640 × 512 pixels, 30Hz, 17mm lens, 9 ft stand-off distance) was used to monitor prefabricated panels subjected to controlled external heating simulating compression molding and resin cure exotherm. Interlaminar delamination defects with characteristic sizes ranging from 0.25 × 0.25in² to 5 × 5in² produced measurable surface temperature depressions of approximately 4–10°C during transient cooling, exceeding the effective noise floor of the camera by more than two standard deviations. Thicker laminates exhibited prolonged defect detectability windows due to increased thermal diffusion time. In contrast, embedded Teflon inclusions generated weak thermal contrasts of ≤ 3°C, approaching the measurement noise floor, due to limited thermal property contrast with the surrounding glass fiber composite. These results establish quantitative detectability limits for stationary thermographic inspection of sandwich composite panels under manufacturing-representative thermal cycles.
This work focused on preferentially aligning discontinuous carbon fibers in wet-laid or air-laid processes. It is well known that aligned fibers provides higher directional strength and stiffness. Discontinuous fibers further allow higher degree of draw and formability as the gaps in the fibers allow for higher material movement. The current processes are limited in their ability to align carbon fibers during processing. The aligned fibers have several benefits - (a) in applications where chopped fibers can replace continuous fibers for targeted strength and stiffness metrics, but at a substantially reduced cost; (b) they can tolerate deeper draws than continuous fiber composites in thermo-stamping and compression molding processes; (c) they can be tailored for pultrusion and unidirectional applications. Although pultrusion is primarily a process that adopts continuous fibers, stitch bonded entangled discontinuous fibers can provide unique intermediates. This is analogous to natural coir fibers which get aligned and entangled to produce ropes/rods for example, (d) they can be processed in cross-ply and multi-directional formats, like composite laminates. In this work Neenah Paper partnered with IACMI, UT and ORNL to evaluate structure-process-property relationships with Zoltek carbon fiber. A few process parameters such as machine speed, weight basis, fiber length, effect of fiber sizing, direction of mat lay-up etc. were investigated. The produced mats were converted to thermoplastic composite laminates using polyamide 6 (PA6, nylon) resin. The specific objective of this project is to produce a wet-laid nonwoven carbon fiber mat with a high degree of unidirectional fiber alignment, using discontinuous carbon fibers. The report provides details about the processing, characterization, and lower-upper bound properties.
Recent major advances in polymer chemistry are enabling a paradigm shift in the area of processing and re-processing/recycling of advanced composite materials. Inexpensive compression molding with short cycle times, traditionally available for thermoplastic composites only, are now possible for the thermoset resins based on polyimine chemistry. Participant will collaborate with the LightMAT consortium Labs ORNL, SNL, and PNNL to non-destructively characterize microscopic structural defects (such as voids and resin-rich areas), and perform high speed impact characterization of its malleable thermoset CFRP's. This work is critical to the validation and adoption of these materials for the automotive market and towards DOE-VTO lightweighting mission objectives.
Kel-F 800 is a copolymer of chlorotrifluoroethylene PTFE (75 wt. %) and vinylidene fluoride PVDF (25 wt. %). It has previously been used as a PBX binder for insensitive explosives such as PBX 9502 and LX-17. 3M started production of Kel-F 800 in 1957 and small-scale batches continued to be made until 2002 when production ceased due to environmental concerns regarding one of the emulsifiers used during production. Around 2000 the Kel-F 800 name was changed to FK-800 to avoid trademark concerns because rights to produce another polymer with a similar tradename (Kel-F 81) had been sold to another manufacturer. The Kel designation came from the original manufacturer of PCTFE (Kel-F 81), the Kellog company. To avoid confusion this document will only refer to Kel-F 800. In 2006, production of small-scale batches of Kel-F 800 was started again by 3M in response to customer enquiries. This new material, the first blended batch is referred to as LOT 1, was produced with a different emulsifier than used previously. Because Kel-F 800 is made in a small batch reactor, considerable variation in crystallinity can be expected from lot to lot and year to year. In many ways, this is not significant since the material is dissolved in a solvent (often MEK, ethylmethyl ketone or ethyl acetate) for PBX production purposes. This destroys the as received crystallinity and the resulting crystallinity in the processed material is a function of polymer molecular weight and thermal history. Producing large billets of Kel-F 800 from solvent extraction is not practical and so a compression molding technique has been used above the melting temperature. This method also removes residual crystallinity from the supplied granules. The molecular weight of a polymer can be estimated by several techniques, the most common being gel permittivity chromatography (GPC), size exclusion chromatography (SEC) and shear rheometry measurements of polymer/solvent solutions. Changes in molecular weight will affect the crystallization rate and the maximum crystallinity reached for a specific thermal history. Both references agree that the new LOT 1 material molecular weight falls within the deviation found from averaging previous historical lots of Kel-F 800.