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This presentation was given at the 2024 AIChE Annual Meeting, San Diego, CA, October 27-31, 2024. The presentation details a method for the efficient fabrication and approximation of membrane performance, developed utilizing 3D printed experimental modules for small hollow fiber modules containing multiple fibers for experimental and simulation comparisons.
Industrial manufacturing of materials may achieve, not only increased profit, but also reduced waste generation, energy consumption, and global greenhouse gas emissions through additive manufacturing (AM). This chapter puts into perspectives the ideas and benefits of using 3D printing technology in the manufacture of durable and sustainable materials, enabling high-value reuse toward the promotion of a better cyclic economy.
Nanocomposites made from alginate and nanoclay are extensively applied for diverse biomedical applications. However, the lack of a clear understanding of the interactions between alginate and nanoclay makes it difficult to rationally design the nanocomposites for different material extrusion-based 3D bioprinting strategies. Here, a combined analytical model is proposed to accurately predict the interaction mechanisms between alginate and nanoclay through small-angle neutron scattering. These mechanisms are summarized into a phase diagram that can guide the design of alginate-nanoclay nanocomposites for different bioprinting applications. The rheological properties of various nanocomposites are measured to validate the proposed interaction mechanisms at the macroscale. Accordingly, three representative extrusion-based bioprinting strategies are linked with the nanocomposite design and applied to freeform fabricate complex structures. In conclusion, a roadmap is summarized to bridge the gap between biomaterial design and bioprinting processes, enabling the rapid and rational selection of biomaterial formula based on available 3D printing methods, and vice versa.
Many liquid metal plasma-facing component concepts for fusion reactors require a capillary porous material to wick the liquid metal to the surface of the component. In this work, samples of 3D-printed molybdenum lattices designed to have pore sizes ranging from 100 to 1000 µm were fabricated by two different suppliers. The dimensions of the lattice structures were characterized using an optical microscope, revealing that the lattice walls were almost systematically thicker than they were designed to be and in turn the pores are all smaller than they were designed to be. In many cases the pores were completely clogged. Several spectroscopic techniques were used to characterize the chemical composition of the materials, collectively indicating the presence of a thick layer of oxygen-rich material extending more than 1 µm below the surface. Compression testing revealed significant asymmetry in the mechanical behavior depending on which direction the force was applied relative to the print direction. Lastly, lithium wetting tests of several lattice samples were performed, and a sample with ~250-µm pores was found to soak up lithium quickly after initial wetting of the surface occurred. The implications of these results for future liquid metal plasma-facing component design are discussed.
Additive manufacturing (AM) enables the fabrication of complex geometries, yet its application to thermosets remains limited by post-processing requirements. Frontal ring-opening metathesis polymerization (FROMP) offers a promising alternative, enabling energy-efficient, in situ curing of freestanding thermoset structures. This study presents a real-time process monitoring and automated control system for direct ink writing (DIW) of FROMP thermosets. By integrating thermochromic leuco dyes and computer vision, we enable real-time polymerization front tracking, allowing autonomous printing parameter adjustments for consistent geometries across resin formulations. The system’s accuracy was validated against manual tracking, demonstrating precise front velocity detection. Its adaptability was confirmed by printing freestanding mechanical springs with different resins, achieving consistent geometries and mechanical properties despite front velocity variations. These findings highlight the potential of automated DIW control for scalable, repeatable, and material-agnostic 3D printing of thermosets.
Lignin is a low-cost and renewable bioresource with a huge annual production promising to prepare sustainable materials. However, the poor interfacial adhesion between many lignin-polymer pairs deteriorates the mechanical performance of the composites, which seriously limits the application of lignin in 3D printing via fused depositional modeling. This work examined lignin-polyamide 12 (PA 12) intermolecular interactions (e.g., hydrogen bonding) to address the interface challenge. To realize this goal, the phenolic hydroxyl content was increased for a kraft softwood lignin using a LiBr/HBr demethylation procedure, increasing phenoxy content by 61.7%. Increased hydrogen bonding interactions between modified lignin (Pine-Lig-OH) and PA 12 demonstrated a significantly improved molten dynamic modulus by rheological analysis. Regarding mechanical properties, by adding 20 wt% of Pine-Lig-OH, the tensile strength and Young's modulus reached 46.6 MPa and 1.62 GPa, 30.2% and 33.9% higher than PA 12, respectively. Further morphological analysis proved the interfacial interactions are enhanced by showing the difference in the phase gaps. The dynamic mechanical analysis (DMA) supported the conclusion that Pine-Lig-OH could interact with polymer chains, alternating segmental movements due to the strong interaction. Here, this study presents a method to enhance lignin composite properties by promoting interactions with the polymer matrix through modified functional groups, guiding future lignin composite research.
The zinc-ion hybrid capacitor is a promising energy storage device, but current overall capacity is limited by the capacitance of the carbon cathode. We have produced a hierarchically porous, nitrogen-doped carbon cathode with good cycling and mechanical stability by 3D printing and pyrolysis of the zinc-based metal–organic framework ZIF-8. When incorporated into a zinc-ion hybrid capacitor, we achieved an areal capacitance of 16.9 F cm -2 and energy density of 7.23 mW h cm -2 , outperforming zinc-ion hybrid capacitors based on conventional cathodes.
Significance Molecular ferroelectrics, which show the ability to switch the electromechanical activity by an external electric field, establish the basis for mechanical metamaterial technologies. Despite their theoretical promise, such mechanical metamaterials remain hindered by the lack of adaptive stimuli-responsive materials which can be effectively tuned “on demand” across time and length scales. Here, we unravel a printable mechanical metamaterial of imidazolium perchlorate with superior electromechanical coupling and reprogrammable stiffness. We propose a continuous rapid three-dimensional (3D) printing technique which can reduce the manufacturing time of ferroelectrics from hours down to minutes. The printed molecular ferroelectric metamaterial structure is then shown to enable a tunable-frequency vibration-isolating architecture. This study paves the way for rationally designed 3D-printable molecular ferroelectric metamaterials.
Oak Ridge National Laboratory (ORNL), in collaboration with mechanical-thermal energy storage (mTES) provider EarthEn, a US Department of Energy (DOE) Lab-Embedded Entrepreneurship Program (LEEP) recipient at ORNL’s Innovation Crossroads 2023, is utilizing a state-of-the-art patented 3D printing technique to design an additively manufactured (AM) supercritical CO2 (sCO2) recuperator (REC) for EarthEn’s charge/discharge cycle. The AM REC will be printed at ORNL’s Manufacturing Demonstration Facility using Inconel Alloy 718 and tested on a closed-loop, ∼100 kW scale experimental facility that is under construction. The testing will compare the printed design against a commercial-off-the-shelf Printed Circuit Heat Exchanger (PCHE) REC. The design of the sCO2 facility is guided by a Modelica-based system model which is primarily dependent on the open-source TRANSFORM library developed at ORNL and uses the open-source CoolProp library for thermophysical properties of sCO2 via the External Media library. It is envisioned that an iterative process will be followed between the physical loop and the system model wherein the initial experimental data will be used to tune the model, which in turn will be used to guide future loop operation. Simultaneously, the AM REC is being designed using computer-aided design models, and it is also being analyzed for hydraulic and thermomechanical response using commercial computational fluid dynamics software, Simcenter STAR-CCM+, on highperformance computing resources.1
Soft-elasticity in monodomain liquid crystal elastomers (LCEs) is promising for impact-absorbing applications where strain energy is ideally absorbed at constant stress. Conventionally, compressive and impact studies on LCEs have not been performed given the notorious difficulty synthesizing sufficiently large monodomain devices. Here, we use direct-ink writing 3D printing to fabricate bulk (>cm 3 ) monodomain LCE devices and study their compressive soft-elasticity over 8 decades of strain rate. At quasi-static rates, the monodomain soft-elastic LCE dissipated 45% of strain energy while comparator materials dissipated less than 20%. At strain rates up to 3000 s –1 , our soft-elastic monodomain LCE consistently performed closest to an ideal-impact absorber. Drop testing reveals soft-elasticity as a likely mechanism for effectively reducing the severity of impacts – with soft elastic LCEs offering a Gadd Severity Index 40% lower than a comparable isotropic elastomer. Lastly, we demonstrate tailoring deformation and buckling behavior in monodomain LCEs via the printed director orientation.
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Additive printing techniques are regarded as revolutionary and versatile methods of advanced device manufacturing, stemming from the possibility to pattern materials on a custom-based approach and the potential to create novel microstructures and achieve new functionalities. Despite these advantages, the inherent anisotropy of the printing process is a source of property gradients within the printed materials, often associated with variable and/or poor performance. Up to date, the evolutionary pathways associated with printing have largely remained unaddressed, mainly owing to the difficulty to study the transformations induced in the material during processing. Time-resolved coherent X-ray scattering techniques, such as X-ray photon correlation spectroscopy, enable the in situ study of transient nanoscale and mesoscale states in a large variety of materials, including amorphous ones, by directly accessing the most relevant timescales and length scales of their nanoscale and mesoscale dynamics, self-assembly, and mesostructure evolution. In this work, we conduct in operando studies of continuous-flow direct writing with colloidal inks, focusing on how the ink formulation and ink-substrate interactions affect the processes that determine the macroscopic properties of the printed materials. We find fundamental differences in the ink structural relaxations emerging from the primary colloid properties (monodisperse versus aggregated colloids) and the substrates surface energy and mechanical properties. Our work helps to reveal and quantify the basic science governing the evolution of 3D-printed materials during processing, ultimately improving engineering criteria for the design of printable materials.
Electrochemical approaches provide unique means to fabricate thin films of metal organic frameworks (MOFs). However, the kinetics of electrochemical MOF deposition has not been quantitatively investigated so far. In this study, we report the first in situ measurements of electrochemical MOF growth using transmission synchrotron X-ray scattering. Electrochemical cells based on poly(lactic acid) with two windows were fabricated using fused-deposition modelling. Here, the resulting 3D-printed cells, the surface of which was coated with paraffin wax to prevent solvent percolation through the polymer material, were used to monitor the cathodic growth of zeolitic imidazolate framework-8 (ZIF-8) on graphite in a methanol solution containing ZnCl 2 and 2-methylimidazole (Hmim) at different cathodic potentials. The resulting time-resolved X-ray diffraction data showed a gradual increase in crystal size with negligible changes in crystal orientation during the cathodic ZIF-8 deposition. More importantly, the time-resolved data provided a means to quantitatively assess the kinetics of the cathodic ZIF-8 growth using the Gualtieri model, revealing that the cathodic potential and Hmim concentration affected crystal growth kinetics, but not nucleation kinetics. These ZIF-8 samples exhibited changes in X-ray diffraction pattern after being washed with methanol and dried in air, indicating that in situ measurements are essential to investigate mechanisms behind MOF electrodeposition.
The overall objective of this proposal was to research, develop, and evaluate a modular direct air capture (DAC) system that is simple and scalable. This system was based on the adsorption of CO 2 into commercial polyamines supported by porous fiber sorbents, which can be produced at kilometer per hour scales using our pre-pilot spinning line. We have housed these fiber materials in novel 3D printed modular housing systems that provide easy-to-manufacture and localized heat integration and flow control. This hybridization of fiber sorbent technology with modular housing provided several advantages that led to lower air pressure drops, higher sorbent productivity, as well as ease of manufacturing and assembly unrivaled by existing and emerging heat integrated contactor designs. The modular housing was fabricated with the following features, at a minimum: (i) a tapered air intake to reduce pressure drop related to entrance effects, (ii) a structured network of heat transfer channels to enable localized cooling and heating during adsorption and desorption, respectively, and (iii) low pressure drop supports for the fiber sorbents. This hybrid manufacturing approach provides a facile method for taking fiber sorbents from lab scale to pilot scale as it dramatically simplifies the fabrication of heat integrated contactor structures.
The practical deployment of lithium–sulfur batteries (LSBs) is hindered by fundamental limitations in conventional slurry-cast cathodes, including poor sulfur utilization, sluggish ion transport, and low areal capacity, particularly in thick electrodes required for high energy density. To address these challenges, we present direct ink writing (DIW) as an additive manufacturing strategy to fabricate advanced current-collector-free, 3D-printed sulfur cathodes (3DP S@CoNi-DSACs/NC) with hierarchically porous architectures that enhance lithium-ion diffusion, promote electrolyte penetration, and reduce interfacial resistance. The synergistic effects of Co/Ni dual-atom sites accelerate redox kinetics and mitigate polysulfide shuttling. As a result, the optimized 3DP cathode with a sulfur loading of 5.4 mg cm −2 demonstrated excellent rate capability, delivering a high reversible capacity of 1041.4 mAh g −1 at 1C with 85.5% capacity retention after 1000 cycles, significantly outperforming its cast counterpart. Remarkably, even at a higher sulfur loading of 8.1 mg cm −2 , the 3DP cathode maintains outstanding performance, achieving a discharge capacity of 1538.4 mAh g −1 and an areal capacity of 12.5 mAh cm −2 at 0.1C. This study not only demonstrates the functional integration of catalytically active materials into 3D printable sulfur cathode architectures but also offers a scalable and transformative platform for building high-performance LSBs beyond conventional electrode manufacturing methods.
Additive manufacturing, particularly fused deposition modeling, is transforming modern production by enabling rapid prototyping and complex part fabrication. However, its layer-by-layer process remains vulnerable to faults such as nozzle clogging, filament runout, and layer misalignment, which compromise print quality and reliability. Traditional inspection methods are costly, time-intensive, and often limited to post-process analysis, making them unsuitable for real-time intervention. In this current study, the authors developed a novel, low-cost, and portable faultdetection system that leverages multimodal sensor fusion and artificial intelligence for real-time monitoring in FDM-based 3D printing. The system integrates acoustic, vibration, and thermal sensing into a non-intrusive architecture, capturing complementary data streams that reflect both mechanical and process-related anomalies. Acoustic and thermal sensors operate in a fully contactless manner, while the vibration sensor requires minimal attachment such that it will not interfere with printer hardware, thereby preserving portability and ease of deployment. The multimodal signals are processed into spectrograms and time-frequency features, which are classified using convolutional neural networks for intelligent fault detection. The proposed system advances Industry 4.0 objectives by offering an affordable, scalable, and practical monitoring solution that improves faultdetection accuracy, reduces waste, and supports sustainable, adaptive manufacturing.
Additive manufacturing techniques enable a wide range of possibilities for novel radiation detectors spanning simple to highly complex geometries, multi-material composites, and metamaterials that are either impossible or cost prohibitive to produce using conventional methods. The present work identifies a set of promising formulations of photocurable scintillator resins capable of neutron-gamma pulse shape discrimination (PSD) to support the additive manufacturing of fast neutron detectors. The development of these resins utilizes a step-by-step, trial-and-error approach to identify different monomer and cross-linker combinations that meet the requirements for 3D printing followed by a 2-level factorial parameter study to optimize the radiation detection performance, including light yield, PSD, optical clarity, and hardness. The formulations resulted in hard, clear, PSD-capable plastic scintillators that were cured solid within 10 s using 405 nm light. The best-performing scintillator produced a light yield 83% of EJ-276 and a PSD figure of merit equaling 1.28 at 450–550 keVee.
LATTICE structures are increasingly used in product design across different industries, including the Department of Energy (DOE), due to their high strength and lightweight properties. These structures possess qualities such as high stiffness, energy absorption, large surface area, and structural support. To ensure lattice structures' quality and symmetry, it is crucial to have defect-free structures. However, in some cases, traditional non-destructive evaluation methods may not be practical due to encasing lattice structures in material. To analyze the lattice structures' quality, this project will employ CT imaging to gain access to the encased structures and perform a detailed analysis of each section. Three 3D printed complex lattice cubes were created, with two exposed and one encased in material, for this project. The CT X-ray cabinet will be used to scan all three cubes, and the data collected will be reconstructed and evaluated using complex interpretation software. This analysis will allow for a detailed examination of the structure's porosity, inclusions, cracks, wall thickness, and symmetry in each section.