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Autoclave processing is a commonly used state-of-the-art fiber-reinforced composite manufacturing technology, albeit with high capital cost, long cycle times and high energy consumption. Alternatively, out-of-autoclave processing reduces the initial and operating costs while producing composite structures with similar quality as that of autoclave parts. Additive Manufacturing (AM) the scaled-up molds for out-of-autoclave process using carbon fiber (CF) reinforced composite offers design flexibility, enhanced mechanical, and thermal properties in addition to reduction in weight and cost. However, heating of these molds using an oven is still expensive and necessitates an energy-efficient heating process. In this study, resistive heating through heating elements embedded within fiber reinforced composite molds is used as an efficient heating mechanism. The goal is to design wire embeddings and determine the optimal heat flux density to achieve a target uniform temperature of 80°C across the mold surface. To this end, numerical analyses were performed to evaluate the temperature distribution across the composite mold surface for a given wire placement and mold configuration. Constant thermal properties of the 20 wt.% short CF reinforced acrylonitrile butadiene styrene (ABS) were used in the thermal analysis. Time taken to reach the steady state temperature was also estimated. Design guidelines for wire embeddings were included to enable efficient manufacturing of fiber-reinforced composites through out-of-autoclave molds.

Plate-based lattices are predicted to reach theoretical Hashin–Shtrikman and Suquet upper bounds on stiffness and strength. However, simultaneously attaining high energy absorption in these plate-lattices still remains elusive, which is critical for many structural applications such as shock wave absorber and protective devices. In this work, we present bi-material isotropic cubic + octet sandwich plate-lattices composed of carbon fiber-reinforced polymer (stiff) skins and elastomeric (soft) core. This bi-material configuration enhances their energy absorption capability while retaining stretching-dominated behavior. We investigate their mechanical properties through an analytical model and finite element simulations. Our results show that they achieve enhanced energy absorption approximately 2–2.8 times higher than their homogeneous counterparts while marginally compromising their stiffness and strength. When compared to previously reported materials, these materials achieve superior strength-energy absorption characteristics, making them an excellent candidate for stiff and strong, lightweight energy absorbing applications. Graphic Abstract: [Figure not available: see fulltext.] Published version

Extrusion based big area additive manufacturing process is utilized for fabrication of dense anisotropic bonded magnets. High loading fraction (≥70 vol%) of magnequench anisotropic Nd–Fe–B powder in nylon is used for preparing anisotropic bonded magnets. A higher energy product of ~143.2 kJ/m3 is obtained for the post printed magnetic field aligned at 1 Tesla. These findings make an important step towards the fabrication of gap magnets with energy product between ferrite and Nd–Fe–B sintered magnets. Moreover, printed bonded magnets exhibited better thermal stability, mechanical properties and superior magnetic properties compared to commercial injection molded magnets.

Carbon fiber (CF)-reinforced thermoplastic composites have been widely used in different structural applications due to their superior thermal and mechanical properties. The big area additive manufacturing (BAAM) system, developed at Oak Ridge National Laboratory’s Manufacturing Demonstration Facility, has been used to manufacture several composite components, demonstration vehicles, molds, and dies. These components have been designed and fabricated using various CF-reinforced thermoplastics. In this study, the dynamic rheological and mechanical properties of a material commonly used in additive manufacturing, 20 wt% CF-acrylonitrile butadiene styrene (ABS), as well as three CF-reinforced high-temperature polymers, 25 wt% CF-polyphenylsulfone (PPSU), 35 wt% CF-polyethersulfone (PES), and 40 wt% CF-polyphenylene sulfide (PPS), used to print molds were investigated. The viscoelastic properties, namely storage modulus, loss modulus, tan delta, and complex viscosity, of these composites were studied, and the rheological behavior was related to the BAAM extrusion and bead formation process. The results showed 20 wt% CF-ABS and 40 wt% CF-PPS to display a more dominant elastic component at all frequencies tested while 25 wt% CF-PPSU and 35 wt% CF-PES have a more dominant viscous component. This viscoelastic behavior is then used to inform the deposition and bead formation process during extrusion on the BAAM system.

Conventional 3D printing approaches are restricted to building up material in a layer-by-layer format, which is more appropriately considered “2.5-D” printing. The layered structure inherently results in significant mechanical anisotropy in printed parts, causing the tensile strength in the build direction (z-axis) to be only a fraction of the in-plane strength – a decrease of 50–75% is common. In this study, a novel “z-pinning” approach is described that allows continuous material to be deposited across multiple layers within the volume of the part. The z-pinning process is demonstrated using a Fused Filament Fabrication (FFF) printer for polylactic acid (PLA) and carbon fiber reinforced PLA. For both materials, z-pinning increased the tensile strength and toughness in the z-direction by more than a factor of 3.5. Direct comparisons to tensile strength in the x-axis showed a significant decrease in mechanical anisotropy as the volume of the pin was increased relative to the void in the rectilinear grid structure. In fact, the PLA sample with the largest pin volume demonstrated mechanically isotropic properties within the statistical uncertainty of the tests. Tensile test results were also analyzed relative to the functional area resisting deformation for each sample.

In this work, we describe an efficient and environmentally benign method of recycling of additive printed Nd-Fe-B polymer bonded magnets. Rapid pulverization of bonded magnets into composite powder containing Nd-Fe-B particles and polymer binder was achieved by milling at cryogenic temperatures. The recycled bonded magnets fabricated by warm compaction of ground cryomilled coarse composite powders and nylon particles showed improved magnetic properties and density. Remanent magnetization and saturation magnetization increased by 4% and 6.5% respectively, due to enhanced density while coercivity and energy product were retained from the original additive printed bonded magnets. This study presents a facile method that enables the direct reuse of end-of-life bonded magnets for remaking new bonded magnets. In addition to magnetic properties, mechanical properties comparable to commercial products have been achieved. This research advances efforts to ensure sustainability in critical materials by forming close loop supply chain.

Phenolic resin was mixed with a cross-linking agent divinylbenzene (DVB) to prepare a polyaniline-based electrically-conductive thermosetting polymer composite. It has been shown that this Phenol-DVB mixture can undergo cationic polymerization in the presence of the dodecylbenzene sulfonic acid (DBSA)-doped polyaniline (PANI). Composites with different weight ratios of phenolic resin and DVB were mixed with a fixed weight of DBSA-PANI (i.e. 30 wt. %). Increasing the phenol content in the resin system was found to improve the electrical conductivity of the composite to almost 2700%. This improvement has been assigned to the reduced de-doping of polyaniline in phenol-DVB resin. Active sites of phenol effectively attached to the β carbon of DVB and reduced the proton subtracting species of DVB, leading to reduced de-doping of PANI. This behavior was studied through various characterization techniques including differential scanning calorimetry (DSC), FT-IR spectroscopy and Scanning Electron Microscopy (SEM). Electrical conductivity measurement, mechanical properties, and in-situ electrical conductivity measurements were performed to find the optimized properties of the composite. Optimized composites prepared with the composition of 30 wt. % DBSA-PANI and 70 wt. % of phenol-DVB (50 wt. % each), have shown electrical conductivity of 0.20 S/cm and a flexural modulus of 2.1 GPa, which is a significant improvement in the flexural properties of polymer based-thermosetting composites with similar electrical conductivity. This material can be a potential candidate for the lightning strike protection of fiber reinforced plastics.

The process simulation tool Additive3D has been developed in Abaqus© 2017 to model the Extrusion Deposition Additive Manufacturing (EDAM) process for fiber-reinforced thermoplastic composites. This additive manufacturing (AM) method encompasses material deposition processes where geometries are constructed layer by layer and the resulting layer properties are highly anisotropic. The goal is to predict final deformed shapes and residual stresses of printed geometries due to the printing process and the material anisotropy. The resulting design tool allows to assess the outcomes of the printing process based on the part geometry, the printing material and the position control parameters. Material properties were characterized, and validation experiments, without additional calibration, show an excellent agreement between modeled and measured part deformation states with relative deviations below 7%. Due to the physics-based nature of the developed simulation tools, the simulations can be extended to account for different part scales, printing materials and printing histories.

The current severe acute respiratory syndrome coronavirus 2 (SARS-COV-2) pandemic has highlighted the need for personal protective equipment, specifically filtering facepiece respirators like N95 masks While it is common knowledge that polypropylene (PP) is the industry standard material for filtration media, trial and error is often required to identify suitable commercial precursors for filtration media production This work aims to identify differences between several commercial grades of PP and demonstrate the development of N95 filtration media with the intent that the industry partners can pivot and help address N95 shortages Three commercial grades of high melt flow index PP were melt blown at Oak Ridge National Laboratory and broadly characterized by several methods including differential scanning calorimetry (DSC), X-ray diffraction (XRD), and neutron scattering Despite the apparent similarities (high melt flow and isotacticity) between PP feedstocks, the application of corona charging and charge enhancing additives improve each material to widely varying degrees From the analysis performed here, the most differentiating factor appears to be related to crystallization of the polymer and the resulting electret formation Materials with higher crystallization onset temperatures, slower crystallization rates, and larger number of crystallites form a stronger electret and are more effective at filtration © XXXX American Chemical Society

Microfibrillated cellulose (MFC) is widely used as a reinforcement filler for biocomposites due to its unique properties. However, the challenge of drying MFC and the incompatibility between nanocellulose and polymer matrix still limits the mechanical performance of MFC-reinforced biocomposites. In this study, we used a water-based transesterification reaction to functionalize MFC and explored the capability of oven-dried MFC as a reinforcement filler for polylactic acid (PLA). Remarkably, this oven-dried, vinyl laurate-modified MFC improved the tensile strength by 38 % and Young's modulus by 71 % compared with neat PLA. Our results suggested improved compatibility and dispersion of the fibrils in PLA after modification. This study demonstrated that scalable water-based surface modification and subsequent straightforward oven drying could be a facile method for effectively drying cellulose nanomaterials. The method helps significantly disperse fibrils in polymers and enhances the mechanical properties of microfibrillar cellulose-reinforced biocomposites.

Until recently, glass fiber composites (GFRP) were the preferred choice to prepare wind turbine blades due to their low cost compared to their counterpart carbon fiber composites (CFRP). However, to harvest the maximum wind energy, ever larger wind turbine blades are being manufactured. To support such a large structure carbon fiber composites CFRP have become the integral part of load bearing structures in the blade. In this work, we are proposing to utilize the low cost carbon fiber (LCCF), manufactured at Carbon Fiber Technology Facility (CFTF) of Oak Ridge National Laboratory (ORNL) as not only the cost effective alternative to the currently used carbon fiber (CF) but also as the lightning strike protection of the wind turbine blades. A textile-grade precursor was used to prepare LCCF. Wind turbines often get hit by lightning strikes due to their operating locations. LCCF can provide structural integrity to these gigantic structures and mitigate the effect of lightning strike on them by effectively dissipating the current. Two composite panels made of LCCF were tested against artificial lightning strikes of 100 kA and 200 kA (component A of lightning

Within the scope of extrusion based additive manufacturing, this chapter provides a review of the research in understanding the physical relationships between microstructure variables and macrostructure properties of high-performance thermoplastic polymers. The development of interlayer strength has been discussed based on the theory of inter-diffusion and re-entanglement of polymer chains at interface. The observations from the study in joining and direct-bonding of polymer surfaces provide insights into the mechanisms of the formation of interface between adjacent layers. Quantitative prediction of interfacial strength as a function of processing temperature and contact time is presented. The mechanisms that lead to reduced mechanical strength at the interface are discussed. The second half of the chapter outlined a set of printing conditions and their influence on structural properties.

Extrusion based high-throughput Additive Manufacturing (AM) provides a rapid and versatile approach for producing complex structures by using a variety of polymer materials. An underexplored aspect of this technique is concerned with the formation of interfaces between successively deposited layers. This is particularly important for large-scale additive manufacturing of semi-crystalline polymers because of the highly non-isothermal conditions involved, which influence both nucleation and crystal growth. The objective of this work is to investigate the microstructure and the corresponding viscoelastic properties of carbon fiber (CF) reinforced polyphenylene sulfide (PPS) resulting from extrusion-based high-throughput AM process. Questions on development of morphology focus on polymer crystal structure and carbon fiber orientation in the vicinity of the interface between successive layers. This study attempts to establish a fundamental understanding of the role of the AM has in transferring a set of intrinsic material properties to the macroscopic properties of the final AM structure.

This article presents a practical model for evaluating polymer feedstock materials as candidates for 3D printing across a variety of extrusion-based platforms. In order for a material to be successfully utilized for 3D printing operations, a series of fundamental conditions must be met. First, pressure-driven extrusion must occur through a given diameter nozzle at a specified flow rate. Second, the extruded material must form and sustain the desired shape. Third, the extruded structure must be able to bridge a specified gap and serve as a mechanically sound foundation for successive deposits. Finally, the deposited structure must be dimensionally stable during the transition to the final state (i.e. fully cured at room temperature). This article presents a framework for extrusion-based printing and a simple viscoelastic model for each of these conditions based on the rheological and thermo-physical properties of the candidate material and the processing parameters of the extrusion-based deposition platform. The model is demonstrated to be a useful tool for the evaluation of example test cases including: high temperature thermoplastics (polyphenylsulfone), fiber reinforced thermoplastics (acrylonitrile butadiene styrene), low-viscosity thermosets (epoxy resins), and thermoplastics with a high coefficient of thermal expansion (polypropylene).

Printing high-performance thermoplastics on large scale extrusion-based additive manufacturing platforms requires stability over a range of processing conditions. However, studies on the melt dynamics and processing conditions of these thermoplastics in big area additive manufacturing (BAAM) are limited. This study characterizes the dynamic rheological behavior of polyetherimide (PEI), a high-performance thermoplastic, as well as carbon fiber (CF)-reinforced PEI composites as a BAAM feedstock material. The viscoelastic properties, such as the storage and loss moduli and complex viscosity, are investigated in relation to the BAAM extrusion process. The results show that CF-PEI composites behave like a viscous liquid during BAAM extrusion. The addition of CF to PEI enhances the shear thinning effect and significantly increases the complex viscosity (2.5× increase for 20% CF, and 3× for 30% CF). The increased viscosity increases the torque on the extruder, which may be alleviated by increasing the material processing temperature.

Recent advancements in the Additive Manufacturing (AM) Fused Filament Fabrication (FFF) approach are described with focus on the application to tooling and molds for composite materials and structures. A detailed summary of mechanical properties of printed parts for different composite material systems is presented and discussed. These material systems are comprised of discontinuous fiber-reinforced polymers characterized by fiber orientation dominantly parallel to the direction of the extrudate. An overview of the FFF process and its physical phenomena is given including the flow and resulting fiber orientation, the bond formation between adjacent beads and the thermomechanical solidification behavior of the deposited material. Based on reviewed research in these different phenomena, future research needs are discussed and desirable objectives are formulated.

As the application space for large-scale 3D printed components continues to grow, it is necessary to identify appropriate processing conditions for high-performance thermoplastics on large format Additive Manufacturing (LFAM) systems. This study compares the rheological behavior of a high-performance thermoplastic, polyphenylsulfone (PPSU), with that of a commonly used low-temperature polymer, acrylonitrile butadiene styrene (ABS), to identify suitable processing conditions for large format AM systems. The linear viscoelastic properties (complex viscosity, storage modulus, loss modulus, and tan delta) of these materials are evaluated as a function of temperature, angular frequency, and carbon fiber content. Over the range of frequencies of interest to LFAM (10–100 rad/s), ABS behaves more like an elastic solid whereas PPSU behaves more like a viscous liquid. The addition of 20–35% by weight of carbon fiber increased the shear thinning effect of both thermoplastics, showing a potential variation of 2–3 x over the range of expected LFAM extrusion shear rates (10–100 s−1).

Magnetically isotropic bonded magnets with a high loading fraction of 70 vol.% Nd-Fe-B are fabricated via an extrusion-based additive manufacturing, or 3D printing system that enables rapid production of large parts. The density of the printed magnet is ∼ 5.2 g/cm3. The room temperature magnetic properties are: intrinsic coercivity Hci = 8.9 kOe (708.2 kA/m), remanence Br = 5.8 kG (0.58 T), and energy product (BH)max = 7.3 MGOe (58.1 kJ/m3). The as-printed magnets are then coated with two types of polymers, both of which improve the thermal stability as revealed by flux aging loss measurements. Tensile tests performed at 25 °C and 100 °C show that the ultimate tensile stress (UTS) increases with increasing loading fraction of the magnet powder, and decreases with increasing temperature. AC magnetic susceptibility and resistivity measurements show that the 3D printed Nd-Fe-B bonded magnets exhibit extremely low eddy current loss and high resistivity. Finally, we demonstrate the performance of the 3D printed magnets in a DC motor configuration via back electromotive force measurements.

While PLA possesses modest to good strength and stiffness, broader application is hindered by its brittle nature. The aim of this study was to develop strong and tough polymeric materials from renewable biomaterials and understand the underlying interactions and mechanisms. Cellulose nanofibrils (CNFs) and epoxidized soybean oil (ESO) were compounded with poly(lactic acid) (PLA) to create a PLA-CNF-ESO tertiary nanocomposite system. Tensile and dynamic mechanical analyses were performed to see how variations in ESO and CNF content affect mechanical properties such as strength, modulus, ductility, and toughness. It was found that at low CNF levels (10 wt%) the addition of ESO can improve the ductility of the nanocomposites 5- to 10-fold with only slight losses in strength and modulus, while at higher CNF levels (20 and 30 wt%), ESO exhibited little effect on mechanical properties, possibly due to percolation of CNFs in the matrix, dominating stress transfer. Therefore, it is important to optimize CNF and ESO amounts in composites to achieve materials with both high strength and high toughness. Efforts have been made to understand the underlying mechanisms of the mechanical behavior of one class of these composites via thermal, dynamic mechanical, rheological, morphological, and Raman analyses.

Carbon fiber reinforced polymer composites (CFPC) have been used in additive manufacturing (AM) due to both the high-strength-to-weight and superior-stiffness-to-weight ratios. CF AM is being considered for tooling applications. In AM, CFPCs are usually aligned along the deposition direction; however, it results in anisotropic thermal properties which affect the heat transfer and warpage of the final part. In this study, three male molds with different infill patterns were produced via the material extrusion additive manufacturing (EDF-AM) process. These include (a) 0°: infill pattern along the printing direction; (b) 90°: infill pattern perpendicular to the printing direction; and (c) 0°/90°: alternate layers along and perpendicular directions. The effect of the infill pattern on thermal conductivity was analyzed and observed that 0° infill (surface temperature: 79.2°C) had the highest conductivity; and 90° infill (surface temperature: 66.4°C) had the least. Highlights (for Review) In Additive manufacturing, carbon fibers are usually aligned along the deposition direction; however, it results in anisotropic thermal properties which affect the heat transfer and warpage of the final part. In this study, three molds with different infill patterns were produced via the extrusion deposition fabrication-additive manufacturing (EDF-AM) process. These include (a) 0°: infill pattern along the printing direction; (b) 90°: infill pattern perpendicular to the printing direction; and (c) 0°/90°: alternate layers along and perpendicular directions. Mold was used for extrusion compression molding and degradation of the mold was analyzed using non-contact laser scanning device.

Large-scale material extrusion additive manufacturing technology is becoming the new mainstream technology for scaled-up composite mold and die applications. This paradigm shift in composite processing technology is primarily driven by out-of-autoclave tooling applications, in which fiber reinforced composite molds with scaled-up sizes and embedded heating elements are attractive. The present research describes the design, manufacturing, and testing of self-heating composite molds fabricated via a large-scale pellet extrusion 3D printing machine with an integrated wire co-extrusion tool. Polycarbonate (PC) composites reinforced with carbon fiber (PC/CF; 20 wt.%) and glass fiber (PC/GF; 20 wt.%) were used to fabricate mold parts. Joule heating thermal test results showed that uniform temperatures (~100 °C) were achieved for both PC/CF and PC/GF mold surfaces, using a custom-made feedback control power supply and infrared thermography. Mechanical characterizations, including tensile and flexural testing were performed on the wire-embedded and un-wired PC/CF and PC/GF base specimens to investigate the impact of the fiber reinforcement as well as the embedded wires. In the direction of extrusion, the ultimate tensile stress of PC/CF was 105 MPa, and that of PC/GF was 73 MPa, while the neat PC value was 64 MPa. Inner-bead voids and interfacial gaps were observed and characterized via optical and scanning electron microscopy. The embedded wires and inner bead impacted the mechanical properties of the composites. However, the stiffness of the wire-embedded mold was still satisfactory, proving that the technology can be used to fabricate additively manufactured out-of-oven/autoclave molds.

As additive manufacturing (AM) continues to develop and become a standardized manufacturing method, there will be a continued need to provide in-situ monitoring during the manufacturing of polymer composite printed components. Thermal residual stress is a primary cause of failures such as interlayer disbonds or delamination, micro cracking, and dimensional instability, which can occur during or after the build. This study reports a novel digital image correlation (DIC) adaptation to monitor thermal residual stresses during the entire print process for large-scale AM. In this work, DIC has been investigated (a) by the natural speckle produced by the polymer surface for correlation, (b) to monitor AM build, and (c) to evaluate the effect of thermal residual stress on warpage of the printed component. The natural speckle pattern of the AM material resulted in a respectable 3.57% error compared to the traditional painted speckle pattern of 3.05% error. DIC measured a 190% increase in vertical displacement at the edge of the wall compared to the center, indicating warpage during AM. This work is a step towards a non-intrusive residual stress measuring technique using DIC for large-scale AM.

3D printing by fused deposition modeling (FDM) is an advanced additive manufacturing technology for making thermoplastic-based structures. Several studies have recently investigated 3D printing of polylactic acid (PLA) with biomass resources like cellulose, hemicellulose, lignin and whole biomass. Such biodegradable composites are better for the environment and can be used to replace non-biodegradable composites in a variety of applications. Therefore, a deep understanding of printing such biocomposites is needed for supporting such manufacturing. Recent developments focused on FDM printing of PLA filled with biomass resources have been critically reviewed to reveal the intricate aspects of manufacturing of such materials and characterization of the changes caused by biomass-based fillers. Properties of high molecular weight PLA, essentials of printing with PLA and conditions for filament extrusion and printing of biocomposites are discussed. Characterization results from mechanical testing, thermal analysis, viscoelastic properties, imaging and spectroscopy are reviewed for understanding the impact of filling biomass resources in PLA by printing. The latter sections discuss applications, upcycling & recycling and future opportunities for biorefineries.