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1. Examining the mass loss and thermal properties of 3D printed models produced by fused deposition modeling and stereolithography under elevated temperatures

   https://doi.org/10.1108/RPJ-01-2022-0007  

   Hsieh, Shu-An; Anderson, Jared L. (June 2022, Rapid Prototyping Journal)

   Purpose This paper aims to study the mass loss of three-dimensional (3D) printed materials at high temperatures. A preconcentration and analysis technique, static headspace gas chromatography-mass spectrometry (SHS-GC-MS), is demonstrated for the analysis of volatile compounds liberated from fused deposition modeling (FDM) and stereolithography (SLA) 3D printed models under elevated temperatures. Design/methodology/approach A total of seven commercial 3D printing materials were tested using the SHS-GC-MS approach. The printed model mass and mass loss were examined as a function of FDM printing parameters including printcore temperature, model size and printing speed, and the use of SLA postprocessing procedures. A high temperature resin was used to demonstrate that thermal degradation products can be identified when the model is incubated under high temperatures. Findings At higher printing temperatures and larger model sizes, the initial printed model mass increased and showed more significant mass loss after thermal incubation for FDM models. For models produced by SLA, the implementation of a postprocessing procedure reduced the mass loss at elevated temperatures. All FDM models showed severe structural deformation when exposed to high temperatures, while SLA models remained structurally intact. Mass spectra and chromatographic retention times acquired from the high temperature resin facilitated identification of eight compounds (monomers, crosslinkers and several photoinitiators) liberated from the resin. Originality/value The study exploits the high sensitivity of SHS-GC-MS to identify thermal degradation products emitted from 3D printed models under elevated temperatures. The results will aid in choosing appropriate filament/resin materials and printing mechanisms for applications that require elevated temperatures. 

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2. Design, synthesis, and characterization of vinyl-addition polynorbornenes with tunable thermal properties

   https://doi.org/10.1039/D1PY01050F  

   Wang, Xinyi; Jeong, Yewon L.; Love, Christopher; Stretz, Holly A.; Stein, Gila E.; Long, Brian K. (October 2021, Polymer Chemistry)

   Unfunctionalized vinyl-addition polynorbornene (VAPNB) possesses many outstanding properties such as high thermal, chemical, and oxidative stability. These features make VAPNB a promising candidate for many engineering applications. However, VAPNB has a small service window between its glass transition temperature ( T g ) and decomposition temperature ( T d ), and it cannot be readily processed in a melt state. In this work, we demonstrate that the service window of VAPNBs can be tailored through the use of norbornene monomers bearing alkyl, aryl, and aryl ether substituents. The vinyl addition homopolymerization and copolymerization of these functionalized norbornyl-based monomers yielded VAPNBs with high T ′ g s (>150 °C) and large service windows ( T d – T g > 100 °C), which are comparable to other commercial engineering thermoplastics. To further establish the feasibility of melt processing, a functionalized VAPNB material with T g = 209 °C and a service window of 170 °C was successfully extruded and molded into bars. Subsequent characterization of the bars by dynamic mechanical analysis (DMA), nuclear magnetic resonance spectroscopy (NMR), and gel permeation chromatography (GPC) revealed only minor signs of polymer degradation. These studies suggest that substituted VAPNBs could be developed into a new class of engineering thermoplastics that is compatible with workhorse melt processing techniques such as extrusion and injection molding, as well as emerging techniques such as extrusion-based 3D printing. 

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3. Strategic cost and sustainability analyses of injection molding and material extrusion additive manufacturing

   https://doi.org/10.1002/pen.26256  

   Kazmer, David; Peterson, Amy_M; Masato, Davide; Colon, Austin_R; Krantz, Joshua (January 2023, Polymer Engineering & Science)

   Abstract Economic and environmental costs are assessed for four different plastics manufacturing processes, including cold and hot runner molding as well as stock and upgraded material extrusion three dimensional (3D) printers. A larger stock 3D printer was found to provide a melting capacity of 14.4 ml/h, while a smaller printer with an upgraded extruder had a melting capacity of 36 ml/h. 3D printing at these maximum melting capacities resulted in specific energy consumption (SEC) of 16.5 and 5.28 kWh/kg, respectively, with the latter value being less than 50% of the lowest values reported in the literature. Even so, analysis of these respective processes found them to be only 2.9% and 3.8% efficient relative to their theoretical minimum energy requirements. By comparison, cold and hot runner molding with an all‐electric machine had SEC of 1.28 and 0.929 kWh/kg, respectively, with efficiencies of 9.9% and 13.6% relative to the theoretical minima. Breakeven analysis considering the cost and carbon footprint of mold tooling found injection molding was preferable at a production quantity of around 70,000 units. Parametric analysis of model inputs indicates that the breakeven quantities are robust with respect to carbon tax incentives but highly dependent on mold costs, labor costs, and part size. Dimensional and mechanical properties of the molded and 3D printed specimens are also characterized and discussed. 

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4. Manufacturing of stereolithographic 3D printed boron nitride nanotube-reinforced ceramic composites with improved thermal and mechanical performance

   https://doi.org/10.1088/2631-6331/acb12a  

   Tank, Mehul; Leon, Ana De; Huang, Wentao; Patadia, Mitesh; Degraff, Joshua; Sweat, Rebekah (January 2023, Functional Composites and Structures)

   Abstract Boron nitride nanotubes (BNNTs) are the perfect candidate for nanofillers in high-temperature multifunctional ceramics due to their high thermal stability, oxidation resistance, good mechanical properties, high thermal conductivity, and radiation shielding. In this paper, 3D printed ceramic nanocomposite with 0.1 wt% of BNNT was prepared by fusing it at high temperatures. Samples were built with three different print directions to study the effect of print layers on mechanical performance along with BNNT addition. Dynamic mechanical analysis is performed to study the length effect of nanoscale reinforcements on the mechanical properties of the printed ceramic composites reporting significant improvements up to 55% in bending strength and 72% in bending modulus with just 0.1 wt% BNNT addition. A 63% thermal diffusivity improvement of ceramic by adding BNNTs is observed using laser flash analysis. The bridging and pull-out effect of nanotubes with a longer aspect ratio was observed with high-resolution microscopy. Such composites’ modeling and simulation approaches are crucial for virtual testing and industrial applications. Understanding the effect of nanoscale synthetic fillers for 3D printed high-temperature ceramics can revolutionize future extreme environment structures. 

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5. High through-thickness thermal conductivity of 3D-printed composites via rotational direct ink writing

   https://doi.org/10.1016/j.addlet.2023.100167  

   Wilt, Jackson K.; Hmeidat, Nadim S.; Bohling, John W.; Compton, Brett G. (December 2023, Additive Manufacturing Letters)

   Composites printed using material extrusion additive manufacturing (AM) typically exhibit alignment of high- aspect-ratio reinforcements parallel to the print direction. This alignment leads to highly anisotropic stiffness, strength, and transport properties. In many cases, it would be desirable to increase mechanical and transport properties transverse to the print direction, for example, in 3D-printed heat sinks or heat exchangers where heat must be moved efficiently between printed roads or layers. Rotational direct ink writing (RDIW), where the deposition nozzle simultaneously rotates and translates during deposition, provides a method to reorient fibers transverse to the print direction during the printing process. In the present work, carbon fiber-reinforced epoxy composites were printed by RDIW with a range of nozzle rotation rates and the in-plane and through-thickness thermal conductivity was measured. In addition, the orientation of carbon fiber (CF) in the composites was measured using optical microscopy and image analysis, from which second-order fiber orientation tensors were calculated. These results showed that the orientation of CF became less anisotropic as nozzle rotation rate increased, leading to increased through-thickness thermal conductivity, which increased by 40% at the highest rotation rate. The orientation tensors also showed that RDIW was more effective at reorienting fibers within the in-plane transverse direction compared to the through-thickness transverse direction. The results presented here demonstrate that a current weakness of material extrusion AM composites—poor thermal conductivity in the through-thickness direction—can be significantly improved with RDIW. 

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