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DOE OSTI2022

Mechanically and Thermally Enhanced 3D-Printed Photocurable Polymer Nanocomposites Containing Functionalized Chitin Nanowhiskers by Stereolithography

Additive manufacturing, or simply 3D printing (3DP), where objects are built through layer-wise material deposition, has gained significant academic and industrial attention as a result of the development of advanced and functional materials requiring rapid, customized, and flexible solutions. In the context of green manufacturing, diversifying environmentally and economically sustainable material portfolios is an essential endeavor for the success of 3DP technology that uses widely available, highly valuable, and renewable materials. Here, we used stereolithography (SLA) for processing methacrylate-based photocurable resins containing crab shell-derived chitin nanowhiskers (CNWs), which are surface-functionalized by reactive acrylate groups. Results from full spectral, thermal, structural, and topological analyses corroborate not only the surface functionalization of CNWs but also indicate the presence of these photocurable CNW (pCNW) fillers in the 3D-printed nanocomposites. Owing to the strong interfacial bond induced by the physical and chemical crosslinking between the pCNW and methacrylate (MA) polymer matrix, the internally formulated nanocomposites displayed enhanced thermomechanical properties (e.g., storage modulus and glass transition temperature) compared to those of commercially available pure SLA resins. For instance, the inclusion of 0.5 wt % pCNW improved the tensile strength and stiffness to up to 78 and 71%, respectively, without compromising the toughness and ductility of the printed material. Accordingly, this result also evidences the compatibility between the filler and resin materials. Consequently, the formation of a crosslinked network in the nanocomposite structure results in a higher thermal stability and activation energy (i.e., up to ~79%) for all the hybrid materials than the pristine MA. Finally, the high-resolution SLA print features, dimensional accuracy, and enhanced mechanical performance of our microstructure-forming functionalized chitin-based nanocomposites make them promising materials for a wide range of robust and high-performance industrial applications.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Simulation of DWPF Chemical Process Cell Using a Reaction Calorimeter

The Defense Waste Processing Facility (DWPF) converts liquid radioactive waste into glass using a Sludge Receipt Adjustment Tank (SRAT) and Slurry Mix Evaporator (SME) in addition to other processes. The SRAT and SME processes can be simulated on a small-scale using the Mettler-Toledo Reaction Calorimeter (RC1). This equipment is able to automate the execution and monitoring of experiments involving nonradioactive chemical simulants. During the chemical processing of sludge in the SRAT process, foam begins to form and can foam over the reaction vessel. The current antifoam used at DWPF creates a risk of increased flammability and has a limited pH range. Usually, mercury is circulated back into the reaction vessel during the SRAT process, making it difficult to remove. To combat foam over, novel antifoams will be tested during the boil-up process using the RC1. To improve mercury extraction, 3D-printed coalescer columns will be tested within the Mercury Water Wash Tank (MWWT) of the RC1. Testing of Simulant Sludge Batch 6 (SB6) was performed to ensure: the sludge would form a stable foam at boiling during full SRAT/SME runs; the antifoam would reduce the amount of foam within the vessel The sludge and a Precipitate Reactor Feed Tank (PRFT) simulant with monosodium titanate (MST) were mixed separately, combined, and then heated to boiling. As shown below, the antifoam used was able to eliminate the foam within the vessel, as expected. The FormLabs Form2 3D Printer can be used to create roughly 3-inch tall and 1-inch diameter columns from clear and ceramic resins. The columns will utilize chemical and physical forces to draw the mercury out of a condensed offgas stream leaving the RC1 reaction vessel. These columns will be tested during full SRAT/SME runs on the basis of how well they are able to collect elemental mercury. In preparation for full-scale runs, the RC1 equipment was assembled onto a custom table and tested with water runs. The software used to control automation, iControl, has a user-friendly interface that allows the experiment to be altered as needed. An example of the data recorded during an experimental run is represented in Figure 1 below. Water runs were utilized as a way to prove if the RC1 system was functioning in the following areas: Boil-up rates, Chemical additions using pumps, Temperature readings, Balance readings, Probe readings, Offgas system, Agitation. Future Plans: Five novel antifoams will be tested during full SRAT/SME runs. The most effective antifoam will be utilized in DWPF's Chemical Process Cell. The design of the Mercury Extraction Coalescer can be further manipulated to increase the extraction of not only elemental mercury, but other heavy metals in environmental remediation processes as well.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

TuFF internal WRAP for Rapid Pipeline Repair (TuFF iWRAP)

The goal of “TuFF internal WRAP for Rapid Pipeline Repair” (TuFF iWRAP) program was to develop a novel material system and placement process to fabricate structural pipe within the existing deteriorated pipelines without disruption of gas delivery. The team (University of Delaware – Center for Composite Materials (UD-CCM) and Plitzie Inc.) addressed this challenge by developing a new material feedstock and pipe in pipe (PIP) repair strategy. This allows the potential for significant cost reduction and has minimum operational impact on gas customers. The new robotic based placement design allows discontinuous placement of pipe sections creating a stand-alone structural liner within the legacy pipeline without the need for pipe shutdown. Here, the material is supplied using a tethered material feeding system and is placed and UV cured with the internal Wound Rapid Automated Placement (iWRAP) system. This provides maximum placement efficiency capable of traversing 90 angle bends in 12-inch pipe and overall design customization to meet pipe repair requirements (e.g., variable wall thickness, bridging gaps, etc.). UV-curable fiber reinforced composite material has been optimized to meet structural performance and placement/cure times. Superior strength and fatigue life has been demonstrated by improving fiber-matrix adhesion using new fiber sizing for UV resins. Rapid cure approaches using new liner and resins have been evaluated with industry. The appropriate design of the section joints has been developed and tested. We estimate coating time to be ~100 hours per mile enabling typical pipe repair within 1 week.

03 NATURAL GAS↗

DOE OSTI2023

Customized Nanostructured Ceramics via Microphase Separation 3D Printing

To date, the restricted capability to fabricate ceramics with independently tailored nano- and macroscopic features has hindered their implementation in a wide range of crucial technological areas, including aeronautics, defense, and microelectronics. In this study, a novel approach that combines self- and digital assembly to create polymer-derived ceramics with highly controlled structures spanning from the nano- to macroscale is introduced. Polymerization-induced microphase separation of a resin during digital light processing generates materials with nanoscale morphologies, with the distinct phases consisting of either a preceramic precursor or a sacrificial polymer. By precisely controlling the molecular weight of the sacrificial polymer, the domain size of the resulting material phases can be finely tuned. Pyrolysis of the printed objects yields ceramics with complex macroscale geometries and nanoscale porosity, which display excellent thermal and oxidation resistance, and morphology-dependent thermal conduction properties. This method offers a valuable technological platform for the simplified fabrication of nanostructured ceramics with complex shapes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Effects of Structure and Filler on Mechanical Properties of Direct Ink Write Pads

Direct ink write (DIW) is an extrusion-based additive manufacturing (AM) technique that enables superior repeatability, property tuning, and material customization compared to conventional manufacturing techniques. In this research, DIW is used to print silicone foams that must accommodate the thermal expansion of other parts. This expansion requires the material to compress and subsequently recover. Thus, a key performance metric is reducing “compression set” or deformation retained after the material is compressed. For this study, a silicone resin was compounded with a getter material, 1,4 bis(phenylethynyl)benzene (DEB) mixed with carbon-supported palladium (Pd) and printed in a variety of lattice structures. The effects of the filler and print structure on compression set were evaluated. In these experiments, 0.5-inch diameter coupons were compressed to 75% their original height for 22 hours at 70 °C, and the change in height calculated at intervals between 30 minutes and 24 hours post-decompression. The unfilled pad with skin layers had the best compression set at 0.7% ± 0.1%, followed by the unfilled pad with no skins at 1.5% ± 0.1%. As the number of filled layers increased, compression set performance degraded. The pad with filled skin layers and all filled layers had a compression set of 7.0% ± 0.3%. Additionally, the reaction extent of DEB was found to increase compression set, possibly due to the diffusion of DEB to the surface at elevated temperatures. Imaging reveals extensive crystallization at the surface. These investigations show that a non-reinforcing filler will increase compression set but that print structure can mitigate this effect.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Additive Manufacturing of Self‐Sensing Carbon Fiber Composites

Carbon fiber-reinforced polymer (CFRP) composites have gained substantial attention across various industries owing to their exceptional mechanical properties and lightweight nature. The emergence of additive manufacturing technologies brings new opportunities to the industry, offering advantages such as design freedom, rapid prototyping, and customization. However, the fabrication of CFRP composites through 3D printing techniques poses challenges pertaining to low resolution and limitations in complex geometry realization. This work introduces digital light processing printing as a versatile, high-resolution method ideal for CFRP composite fabrication. Furthermore, the development and characterization of CFRP are focused on and the manipulation of mechanical properties through variations in matrix resins and fiber loadings is investigated, showcasing the versatility of CFRP composites for tailored applications. Additionally, the integration of self-sensing capabilities in CFRP structures is explored, which opens up opportunities for applications in smart components for automotive and structural health monitoring.

carbon fiber composites↗

DOE OSTI2026

Cost-Benefit Assessment of Additive Manufacturing for Injection Molds

This report presents an additive-manufacturing (AM) technology, where AM Cyclic Olefin Resin (COR) molds would be used for injection molding. The National Laboratory of the Rockies (NLR) team has focused on the costs and economics of this developing technology. This report presents a cost-benefit analysis of using the polySpectra AM COR molds made of COR, at the start of the project (Present') and the potential lifetime, cost-effectiveness, and performance by the end of the project period (Period 3'). The analysis of the AM COR molds is compared to traditional Computer Numerical Control (CNC) machined aluminum molds across the time periods. A cost-benefit model framework has been developed to evaluate AM COR molds. This model accounts for mold delivery to customers, current and future levels of technology readiness, the type of material injected, and various business cases. AM COR molds offer a major advantage in lead time, reducing production setup from weeks or months (with CNC machining) to as little as two to five days. This enables faster prototyping, quicker design cycles, and accelerated time-to-market, critical in industries like electronics, aerospace, medical devices, and automotive. Even modest improvements in the durability of polySpectra AM COR molds show the potential for these molds to complement traditional tooling. With further development, AM COR mold technology could provide significant time and cost savings while supporting increased domestic manufacturing capacity.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

DOE OSTI2024

Recent and future developments in pultrusion technology with consideration for curved geometries: A review

Herein this paper examined the current state and future developments in pultrusion with particular emphasis on its application in curved part manufacturing. The relationship between factors such as resin chemistry, fiber characteristics, and die geometry that influences the properties of pultruded product were highlighted. Moreover, the specific challenges associated with pultruding curved parts such as the complexities in achieving uniformity and structural integrity in such geometries were discussed. The review emphasized mold design, process improvement, adaptive control systems for precise resin impregnation and material selection to address these challenges. Additionally, the paper suggests the integration of real-time monitoring and data analytics as ways to enhance quality control during curved parts pultrusion. These advancements will help to overcome challenges specific to curved pultrusion and make the process more efficient. Other manufacturing techniques such as filament winding, thermoforming, pulforming were mentioned as alternatives to curved parts pultrusion. The review also explores pultruded variable curvature processes, highlighting some notable patents and article related to this subject matter. Production of pultruded variable curvature parts was seen as a key driver that can shape the future of pultrusion. Finally, the paper anticipates future trends, with sustainability, customization, integration of advanced materials, and development of techniques for pultrusion of composites parts.

42 ENGINEERING↗