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Here, we report carbon-supported Ni-nanoparticles as reusable catalysts for reductive amidation of nitro compounds with polylactic acid (PLA).
Stable and efficient X-ray scintillators are crucial for medical diagnostics, industrial, and defense applications. However, conventional scintillator technologies face a trade-off between stability, optimal performance, and sustainability. Herein, we introduce 3D-printed Cs 4 MnBi 2 Cl 12 (Pero1) and Cs 4 Cd 0.68 Mn 0.32 Bi 2 Cl 12 (Pero2) perovskite microcrystals embedded within a polylactic acid (PLA) polymer composite as X-ray scintillators, combining efficiency, stability, and sustainability. The orange luminescent perovskite powder phosphors exhibited poor water stability, which was successfully addressed through incorporation into PLA via filament extrusion and fused deposition modeling (FDM) 3D printing. The resulting composite films demonstrated remarkable water stability while maintaining uniform orange emission throughout the polymer matrix, as confirmed by 3D topography scanning and X-ray fluorescence mapping. Structural characterization revealed minimal chemical interaction between the perovskite and PLA matrix, with the composites retaining their crystalline properties. The PLA-Pero2 composite exhibited superior optical properties, with a photoluminescence quantum yield of 47%, nearly 17 times higher than that of PLA-Pero1 (2.8%), attributed to the effective suppression of non-radiative decay pathways through Cd 2+ doping. Under hard X-ray irradiation at synchrotron beamlines, both composites exhibited excellent radioluminescence, with emission peaks at 605 nm, a linear response across a wide X-ray flux range, and remarkable radiation stability, showing less than 3% intensity degradation after 600 seconds of continuous high-dose exposure. The PLA-Pero2 composite achieved a spatial resolution of 5 line pairs per millimeter and a contrast ratio of 0.255. These performance metrics, combined with the polymer's biodegradability and scalability through additive manufacturing, position PLA-based composites as a more sustainable alternative to conventional petroleum-based polymer scintillators for next-generation medical imaging, radiation monitoring, and industrial radiography applications.
Transporting and assembling large, complex structures poses significant challenges due to their size, geometry, and cost. Additionally, the installation sites are often inaccessible or hazardous for humans, necessitating self-assembling capabilities in these structures. To mitigate these challenges, we propose using 3D printing materials with shape memory effect (SME) for both transport and construction. This approach involves developing 3D modular components into flat sheets for easier transportation, and then self-assembling into 3D structures on-site using solar energy. To gain a deeper understanding of the factors influencing material memory performance, we have chosen a composite PLA/WF, which is polylactic acid (PLA) with 20 wt% wood flour (WF) for this purpose, leveraging its high tensile modulus at 0.966 GPa, low cost, and sustainability. Printed shapes with this material can maintain a recovery ratio over 90% after 3 cycles. While traditional composites fillers (e.g. glass or carbon fiber) are added to enhance mechanical and thermal properties, the addition of bio-based fillers like WF accomplish similar goals without compromising sustainability. We conducted multiple experiments to demonstrate how environmental conditions (i.e. temperature) maximize the material’s SME. Although still at an early stage, this study provides initial insights into bridging the gap between the small-scale nature of shape memory polymers (SMPs) and their potential for large-scale additive manufacturing, addressing a critical need for efficient and sustainable construction. In the long term, we hope our study contributes to the design vision of utilizing SMPs for transportation, assembly, and deployment of complex structures, providing a new pathway for sustainable construction and transportation of large-scale structures to hard-to-access locations such as disaster-affected areas and remote deserts, etc.
A high-performance, compact microwave absorber was created using Fused Deposition Modeling (FDM) 3D printing. Both a narrowband and a broadband absorber were created. The narrowband absorber was designed at 4.9 GHz, mid-band in WR-187 waveguide. The broadband absorber tried to achieve the best attenuation across the entire 3.95 to 5.85 GHz band. Two types of carbon loaded polylactic acid (PLA) plastic and one type of unloaded PLA were 3D printed with variable percentages of air to achieve different values of effective dielectric constant and loss tangent. The absorber comprised five or six rectangular pieces of these plastic materials. The thickness and fill factor values for each piece were optimized to minimize reflection through fast analytic modeling in MATLAB®. The results were then verified by HFSS® simulation as well. The stack progressed from the lowest loss and lowest dielectric constant to the highest at the shorting end. The final narrowband load had simulated return loss of 87 dB at 4.9 GHz with an analytic solution in MATLAB. The measured return loss of the 3D printed attenuator was 73 dB at 4.929 GHz. The total length of the absorber was 2.44 inches. A commercial absorber for WR-187 with return loss of 40 dB has length of 13 inches. The experiment proves that an effective and compact microwave absorber can be created using 3D printing.
Here, we present experimental verification of pulse shaping in elastic metamaterials together with a procedure to design, fabricate, and verify metamaterial pulse shapers under impact excitation. The split Hopkinson pressure bar (SHPB) test, a fundamental dynamic test introduced more than 70 years ago, often incorporates pulse shaping as a means to alter a stress wave, providing the primary motivation for the presented study. Elastic metamaterials hold promise for enhancing conventional pulse shaping abilities and improving capabilities of the SHPB test. We first design the pulse shaper by numerically optimizing its response using finite element analysis. The pulse shaper consists of repeated unit cells based on a combination of a phononic crystal and a local resonator. Then, we fabricate and test pulse shaper candidates to validate the procedural efficacy. An iterative element corrects inaccuracies in input force and material properties and allows convergence on an appropriate pulse shaper. We carry out this procedure by designing pulse shapers fabricated from 3D-printed polylactic acid (PLA) to achieve an extended dwell acceleration pulse shape. In experimental impact tests, the procedure results in rise, dwell, and fall behaviors comparable to that predicted, effectively confirming the efficacy of the presented procedure and verifying the performance of metamaterial-based pulse shapers.
This data set contains images produced to test the performance of anomaly and fault detection methods in the context of additive manufacturing. Two print jobs were executed using the Ingersoll MasterPrint with the Model 30 Strangpresse extruder. The material used was Techmer compounded polylactic acid (PLA) with wood flour as a filler (80/20 PLA/WF by weight). The first print job consists of the 3D printing of a hexagonal cylinder with a two-bead wall. This print was sliced at a gantry velocity of 3000 millimeter per minute, and an extruder screw speed of 68.14 rotations per minute. This are considered the normal operating conditions. A second hexagonal cylinder was printed using a reduced extruder screw speed, 15% lower than under normal operating conditions. The images were collected with a Teledyne FLIR Lepton 3.5 infra-red camera, a small form factor radiometric long-wave infrared camera with a spectral range of 8 µm to 14 µm. Sensor resolution was 160x120 pixels, with a pixel size of 12 µm, a temperature range of -10 - 450°C, and an accuracy of +/- 10°C in its low gain configuration. Images in this data set were collected with cameras oriented at the printer nozzle. The nozzle camera setup consisted of two cameras located 12.5cm from the nozzle center. These were mounted directly to the print head, so that the camera positions relative to the print direction would remain constant as it rotated around its C-axis to follow the print path. One camera was placed ahead of the nozzle to capture the previous layer immediately before being covered by the new layer of material, while the second camera was placed behind the nozzle and captured the freshly extruded bead. Images are collecting during each phase of the print: (a) idle (i.e., no material deposited), (b) extrusion (i.e., to prime the extruder), and (c) printing (deposition of material to manufacture the hexagonal cylinder).
This data set contains images produced to test the performance of anomaly and fault detection methods in the context of additive manufacturing. A total of 10 print jobs were executed using a Cincinnati BAAM (model 606) with a Cincinnati medium compression screw. The material used was compounded polylactic acid (PLA) with wood flour as a filler produced by Jabil (80% NatureWorks Ingeo 6060D amorphous PLA, % 100 mesh pine flour from American Wood Fiber). Print sheets were 1/4in polycarbonate.
Polylactic acid (PLA) microspheres are primarily used in drug delivery applications and rarely manufactured commercially. In encapsulation, the drug encapsulation and microsphere synthesis process happen simultaneously. Simultaneous synthesis necessitates conditions that ensure the drugs to be encapsulated remain viable in the synthesis process. Here, in the present work, solid pure PLA microspheres are prepared using a repeatable centrifugal mixing method to create a single emulsion system. A planetary thinky mixer is used to achieve centrifugal mixing. PLA acts as the dispersed phase of the emulsion, whereas Polyvinyl alcohol (emulsifier) dissolved in deionized water serves as the bulk phase. The emulsions are stirred for about 4 min at 2000 rpm. Microspheres prepared by mechanical mixing are compared with microspheres prepared by centrifugal mixing. The microspheres prepared by centrifugal mixing proved to be narrower and closer to a normal distribution with a mean size (D x 50) of 30 microns. The size distribution of planetary mixed microspheres did not change from one batch to another.
Porosity in polymer parts could improve mechanical properties while reducing weight and density. Individual pores must be small enough that bulk mechanical properties are retained but significant enough to reduce the density of the material. Filler materials can be incorporated into polymer matrices and removed to create voids. Here, this paper focuses on creating spherical pores in silicone matrices by inserting and removing core materials or fillers during post-cure. A method was developed to incorporate pore formers into an uncured polymer resin and remove the pore former materials from the matrix. Polyethylene glycol (PEG) and polylactic acid (PLA) microspheres were created and incorporated into silicone matrices as pore formers. Microspheres with controllable size distributions were formed via an emulsion formation. Microspheres are removed from the matrix by solvent extraction and calcination. Thermogravimetric Analysis (TGA), Dynamic Mechanical Analysis (DMA), and optical imaging characterize and determine the successful creation of micropores in the polymer matrices.
Flow control within a particle-based Concentrated Solar Power (CSP) system is essential in determining the heat transfer coefficient, and therefore, the power generation capability of these systems. There are three areas where particle flow control is significant: the receivers, storage tanks, and particle-sCO2 heat exchangers. The focus of this work is on designing a new mechanism to control the flow in the particle-sCO2 heat exchangers due to the simplicity and potential cost savings when compared to the other areas of interest. The goal is for this new design to have quicker response times in terms of particle flowrate than a slide gate or flow control valve, which are designs currently used. The design resembles that of a chuck mechanism within a drill where a rotation of the sleeve elicits movement of the jaws both vertically and horizontally to close the outlet area of the nozzle. Additionally, this design will utilize the current actuator that is already used within these heat exchangers to reduce the complexity of implementation. The jaws are designed to be closed at an angle of 76˚ which is just slightly steeper than the hopper leading to the mechanism. Furthermore, this design can be tuned to limit particle bridging and other particle flow phenomena that result in blockages. The prototypes were 3D printed out of polylactic acid (PLA) and scaled up to 100%, 200%, and 400% to be able to observe the velocity profiles of the mechanism more clearly. Experiments are performed with this prototype to compare the inlet and outlet mass flow rates at different configurations of the jaws. The particles used in these experiments are 0.3mm HSP 40/70 that are commonly used in particle-based CSP systems.
Oak Ridge National Laboratory (ORNL) worked with Mitsubishi Chemical America, Inc. to develop a highly biodegradable ~100% biobased feedstock for large format additive manufacturing (AM). Together, they developed an AM feedstock based on the biobased polyester, polybutylene succinate (PBS), that is typically used in agriculture and packaging projects. The motivation for this work was to leverage the high degradability of this polymer in AM to create a new avenue for end-of-life disposal of the product. A composite feedstock was developed from PBS, polylactic acid (PLA), and wood flour (WF). While WF improves printability, reduces feedstock cost, and can improve stiffness, it also often results in a loss in tensile strength which can inhibit/limit applications of the material. To recover the loss in tensile strength suffered by including large quantities, up to 30 wt.% WF in the composite, a chain extender was used to compatibilize the different composite constituents with each other. The feedstock was used to 3D-print a demonstration mold for precast concrete catch basins and was tested by casting 750 lbs of concrete. The mold survived the demonstration. Aerobic degradation testing of the composite feedstock showed that it was highly degradable, 40% biodegradation after 90 days, compared to other incumbent biobased feedstocks.
Oak Ridge National Laboratory (ORNL) worked with Mitsubishi Chemical America, Inc. to develop a highly biodegradable ~100% biobased feedstock for large format additive manufacturing (AM). Together, they developed a AM feedstock based on the biobased polyester, polybutylene succinate (PBS), that is typically used in agriculture and packaging projects. The motivation for this work was to leverage the high degradability of this polymer in AM to create a new avenue for end-of-life disposal of the product. A composite feedstock was developed from PBS, polylactic acid (PLA), and wood flour (WF). While WF improves printability, reduces feedstock cost, and can improve stiffness, it also often results in a loss in tensile strength which can inhibit/limit application of the material. To recover the loss in tensile strength suffered by including large quantities, up to 30 wt%, WF in the composite a chain extender was used to compatibilze the different composite constituents with each other. The feedstock was used to 3D-print demonstration mold for precast concrete catch basins and was tested by casting 750 lbs of concrete. The mold survived the demonstration. Aerobic degradation testing of the composite feedstock showed that it was highly degradable, 40% biodegradation after 90 days, compared to other incumbent biobased feedstocks.
Cellulosic fibers can impart many unique benefits into composite applications, such as reduced weight or structural reinforcement; however, these materials also increase hygroscopicity and decrease thermal stability, restricting broader applications. The present work adapted an experimental process for functionalizing the cellulose surface using citric acid (CA) for three fibers: a 100% cellulose bleached soft Kraft pulp (e.g., creafill) and two natural fibers with similar composition but different fiber morphology, flax fiber and banana fiber. The process uses CA with a sodium hypophosphite (SHP) catalyst to chemically functionalize fiber surfaces, and the reaction mechanism was investigated through Fourier Transform Infrared Spectroscopy (FTIR), which suggested a grafting mechanism rather than a surface-based crosslinking between neighboring sites. Functionalized fibers were compounded into polylactic acid (PLA) at 20 wt.% to better understand how this functionalization might impact critical performance properties like thermal stability, crystallization, thermal mechanical properties, and water uptake of these composites. The study demonstrated varying levels of efficacy for the functionalization of cellulosic fibers with CA/SHP and the fiber with the most open microstructure, e.g., banana fiber, exhibited the largest change in its properties with a 38% reduction in water uptake compared to untreated banana fiber composites. Parallel evaluation of the functionalization process for different fibers demonstrates the importance of fiber morphology on surface modification and can enable their use in composites by demonstrating the efficacy of this potentially low-cost, low-toxicity method for reducing hygroscopicity and improving thermal stability.
The push for sustainability in all facets of manufacturing has led to an increased interest in biomass as an alternative to non-renewable materials. Hemp bast fiber mats were produced from a bacterial retting process, named BFM, as the fiber reinforcement. The objective of this study was to evaluate the feasibility of laminating BFM with polylactic acid (PLA) for a composite panel product. Since both BFM and PLA are biodegradable, the resulting BFM-PLA composites will be 100% biodegradable. PLA pallets were processed into thin polymer sheets which served as the matrix. The BFM and PLA plates were laminated in five layers and compression-molded into composite panels. Experiments were conducted on the three BFM-to-PLA ratios (35/65, 45/55, and 50/50). Mechanical properties (tensile and bending properties) and physical properties (thickness swell and water absorption) were tested and compared to the currently commercial sheet molding compound (SMC) from fiber glass. The thermal behavior of the BFM/PLA composites was characterized using dynamic mechanical analysis (DMA) and differential scanning calorimetry (DSC). The developed BFM/PLA composite product is a sustainable alternative to existing synthetical fiber-reinforced polymer (FRP) that is biodegradable in landfill at the end of life.
The integral process of depositing thin layers of material, one after another, until the designed component is created is collectively referred to as Additive Manufacturing (AM). Fused deposition process (FDP) is a type of AM where feedstock is extruded into filaments which then are deposited by 3D printing, and the solidification occurs during cooling of the melt. Currently, complex structures are being fabricated by commercial and open source desktop 3D printers. Recently, metal powder containing composite filaments based on polylactic acid (PLA) and acrylonitrile butadiene styrene (ABS) have emerged, which could be utilized for multifunctional applications. For further deployment in the field, especially for aerospace and ground-based applications, it is critical to understand the tribological behavior of 3D printed materials. In this presentation, we will report the tribological behavior of different polymer matrix composites fabricated by fused deposition process. These results will be compared with the base polymer systems. During this study, the tribological behavior of all the samples will be evaluated with tab-on-disc method and compared for different metallic powder reinforcements.
There is a critical need for high performance materials for functional and space-based applications, including tires for exploratory rovers and external structures for landing vehicles. Novel ternary borides, such as iron aluminum boride (Fe2AlB2) and molybdenum aluminum boride (MoAlB), have emerged as potential materials for such application owing to their hardness, mechanical behavior and oxidation resistance. In this poster presentation, we will present different methods of fabricating these particles and engineering them for additive manufacturing and other related manufacturing practices. As an integral component of this study, we will demonstrate technologies to (a) synthesize these particles and (b) microencapsulate these particles with bioplastics like polylactic acid (PLA). The resulting particles will be evaluated for their processability as coatings on hydroxyapatite and Inconel particles using microstructural and flowability studies. It is expected that these particles can be used for 3D printing.
NASA’s Artemis Program seeks to establish a long-term presence on the moon to enable scientific discoveries and utilization of lunar resources through public-private partnerships. Over the next decades, a lunar spaceport enabling regular transportation from and to Earth will need to be established to provide the services and facilities that are necessary to achieve this goal. Robotic construction technologies using in-situ materials must be developed to build up enabling infrastructure such as launch/landing pads, blast protection, power/communications towers, improved trafficability pathways and radiation protection shelters. Kennedy Space Center’s Granular Mechanics and Regolith Operations laboratory at Swamp Works has partnered with AI SpaceFactory to develop the architectural and structural design of an unpressurized shelter. The shelter, called Lina, is designed to protect astronauts and surface assets from radiation, meteoroid impact, moon quakes and thermal gradients. Lina’s structural design criteria and the resulting structure design are detailed in separate papers. A Fused Filament Fabrication (FFF) construction process using regolith polymer composites has been developed. This paper presents the material formulations and selection rationale for each of the composite components. Formulations include 70:30, 80:20, and 85:15 wt.% mixture ratios of lunar mare simulant Black Point-1 (BP-1): Polylactic Acid (PLA), 80:20 Lunar Highlands Simulant (LHS-1): PLA and an 80:20 BP-1:PLA formulation with a processing aid/compatibilizer additive. Test samples were printed in simulated lunar dirty thermal vacuum conditions (~-180 °C, ~10 -3 torr). The test environment evolved throughout the duration of the print process. A series of tests were performed to characterize the mixture ratios achieved for each formulation, the off-gassing products during vacuum printing, the strength properties, and porosity of printed products. The LHS-1: PLA formulation yielded an advantageous combination of properties and was used in a final test that additively constructed a sub-scaled Lina on regolith simulant in dirty vacuum conditions.
NASA’s Artemis Program seeks to establish a long-term presence on the Moon to enable scientific exploration and expand the cis-lunar economy by utilizing lunar resources through public-private and international partnerships. Over the next decades, a lunar spaceport will need to be established to provide the services and facilities that are necessary to achieve this goal. Robotic construction technologies using in-situ materials must be developed to build up enabling infrastructure such as launch/landing pads, blast protection, power/communications infrastructure, improved roads, improved operational surfaces, and radiation protection shelters. Kennedy Space Center’s Granular Mechanics and Regolith Operations laboratory at Swamp Works has partnered with SpaceFactory and LERA Consulting Structural Engineers to develop the architectural and structural design of an unpressurized lunar shelter. The shelter, called Lunar Infrastructure Asset (LINA), is designed to support 2.3 m of regolith overburden to protect astronauts and surface assets from radiation, meteoroid impact, thermal gradients/cycling, and to withstand moonquakes. LINA’s structural design criteria and the resulting structure design are detailed in separate papers. A Fused Filament Fabrication (FFF) construction process using regolith polymer composites has been developed and is detailed in a separate publication. This paper presents material formulations and selection rationale for each of the composite components that were examined. Formulations include 70:30, 80:20, and 85:15 wt.% mixture ratios of lunar mare simulant Black Point-1 (BP-1): Polylactic Acid (PLA), 80:20 Lunar Highlands Simulant-1 (LHS-1): PLA and an 80:20 BP-1: PLA formulation with a flow enhancer additive. Test samples were printed in simulated lunar dirty thermal vacuum conditions (-190 °C, 10-3 torr). A series of tests were performed on each formulation to characterize the achieved mixture ratio, mechanical strength properties, off-gassing products during vacuum printing, and porosity and density of printed products. The LHS-1: PLA formulation yielded an advantageous combination of properties and was used in a final test that additively constructed a sub-scaled LINA on regolith simulant in dirty vacuum conditions. The materials and construction process presented in this paper are considered to be at Technology Readiness Level (TRL) 5 with additional testing necessary to characterize long term lunar environmental exposure effects.