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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Self-terminating etching processes for post-processing of 3D printed metal alloys

A process is provided to remove a selective amount of material from a metal part fabricated by additive manufacturing in a self-terminating manner. The process can be used to remove support structures and trapped powder from a metal part as well as to smooth surfaces of a 3D printed metal part. In one embodiment, selected surfaces of the metal part are treated to make the selected surfaces at least one of mechanically and chemically unstable. The unstable portion of the metal support can then be removed chemically, electrochemically, with a pressure differential, and/or through vapor-phase etching. In one embodiment, the metal part may comprise one or more of an aluminum alloy, a titanium alloy, and a copper alloy. The process can be used to modify any fluid or vapor-accessible regions and surfaces of a 3D printed metal part.

Hildreth, Owen J.↗
DOE OSTI2020

Ink-substrate interactions during 3D printing revealed by time-resolved coherent X-ray scattering

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.

36 MATERIALS SCIENCE↗
DOE OSTI2021

From casting to 3D printing geopolymers: A proof of concept

The objective of this paper is to define a mix design strategy allowing the implementation of geopolymer in powder bed 3D printing. In a selective binder approach, an aluminosilicate powder bed is activated through the deposit of an alkaline silicate solution. We first show that, in comparison to casting, this technology requires mastering the spreading of the liquid into the powder bed to ensure that the reaction takes place where it is needed. A series of experiments at the drop level, mimicking the 3D printing process, were performed to determine the printing solution composition for a given powder bed packing. We then highlight the relationship between the compressive strength of the printed geopolymer and the powder bed saturation, controlled by the printing parameters. Finally, SEM/EDX analysis confirm the formation of geopolymer with desired Si/Al and Na/Al ratios in the resulting printed material.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Alumina-based filters made via binder jet 3D printing of alumina powder, colloidal silica infiltration, and sintering

Alumina-based, porous filter media was made via a binder jet 3D printing process consisting of an alumina powder printing step with subsequent heating, colloidal silica infiltration, drying, and sintering to consolidate particles yet retain a net open porous microstructure. The composites made were alumina-silica or alumina-mullite, where the silica sintering aid was used to densify and join the alumina particles. The resulting composite structures had open porosities in the 25–31 vol% range as measured by Archimedes density. Pressure drops were measured across the filter media at constant flow rates to compare disc shapes and complex, 3D printed filters based on the N95 design requirements. Complex, 3D-printed alumina composites were produced with acceptable pressure drops for N95 implementation.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Mass spectrometric investigations into 3D printed parts to assess radiopurity as ultralow background materials for rare event physics detectors

The mass concentrations of 232 Th and 238 U in several 3D printing filaments and printed polymer parts are reported as measures of their radiopurity. In order to minimize background signals in rare event physics detectors, radiopure polymers are necessary as dielectric and structural materials in their construction. New data are reported for polyvinylidene fluoride (PVDF), polyphenylene sulfide (PPS), and two forms of polyetherimide (PEI, branded ULTEM 1010 and 9085). Data for starting filaments and both simple and complex printed parts are reported. PVDF filaments and simple printed beads, were found to have values of approximately 30 and 50 pg g -1 for 232 Th and 238 U, respectively, while a more complex spring clip part had slightly elevated 232 Th levels of 65 pg g -1 , with 238 U remaining at 50 pg g -1 . PPS filament was found to have concentrations of 270 and 710 pg g -1 for 232 Th and 238 U, respectively, and were not chosen to be printed as those levels were already higher than other material options. ULTEM 1010 filaments and printed complex spring clip parts were found to have concentrations of around 5 and 7 pg g -1 for 232 Th and 238 U, respectively, illustrating no significant contamination from the printing process. ULTEM 9085 filaments were found to have concentrations of around 9 and 5 pg g -1 for 232 Th and 238 U, respectively, while the printed complex spring clip part was found to have slightly elevated concentrations of 25 and 7 pg g -1 for 232 Th and 238 U, respectively. All these results were obtained using a novel dry ashing method in crucibles constructed of ultralow background electroformed copper or, when applicable, microwave assisted wet ashing digestion. Samples and process blanks were spiked with 229 Th and 233 U as internal standards prior to dry/wet ashing and determinations were made by inductively coupled plasma mass spectrometry (ICP-MS). In order to maintain high radiopurity levels, pre-cleaning the filaments before printing and post-cleaning the parts is recommended, although the printing process itself has shown to contribute very minute amounts of radiocontaminants.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

Direct observation of pore formation mechanisms during LPBF additive manufacturing process and high energy density laser welding

Laser powder bed fusion (LPBF) is a 3D printing technology that can print parts with complex geometries that are unachievable by conventional manufacturing technologies. However, pores formed during the printing process impair the mechanical performance of the printed parts, severely hindering their widespread application. Here, we report six pore formation mechanisms that were observed during the LPBF process. Our results in this study reconfirm three pore formation mechanisms - keyhole induced pores, pore formation from feedstock powder and pore formation along the melting boundary during laser melting from vaporization of a volatile substance or an expansion of a tiny trapped gas. We also observe three new pore formation mechanisms: (1) pore trapped by surface fluctuation, (2) pore formation due to depression zone fluctuation when the depression zone is shallow and (3) pore formation from a crack. The results presented here provide direct evidence and insight into pore formation mechanisms during the LPBF process, which may guide the development of pore elimination/mitigation approaches. Since certain laser processing conditions studied here are similar to the situations in high energy density laser welding, the results presented here also have implications for laser welding.

42 ENGINEERING↗
DOE OSTI2021

3D printable feedstock inks for signal control or computation

A 3D printable feedstock ink is disclosed for use in a 3D printing process where the ink is flowed through a printing nozzle. The ink may be made up of a non-conductive flowable material and a plurality of chiplets contained in the non-conductive flowable material in random orientations. The chiplets may form a plurality of percolating chiplet networks within the non-conductive flowable material as ones of the chiplets contact one another. Each one of the chiplets has a predetermined circuit characteristic which is responsive to a predetermined electrical signal, and which becomes electrically conductive when the predetermined electrical signal is applied to the ink, to thus form at least one conductive signal path through the ink.

Murialdo, Maxwell↗
DOE OSTI2021

3D printing of biomedically relevant polymer materials and biocompatibility

Research on polymer materials for additive manufacturing technology in biomedical applications is as promising as it is numerous, but biocompatibility of printable materials still remains a big challenge. Changes occurring during the 3D-printing processes itself may have adverse effects on the compatibility of the completed print. Furthermore, this prospective will put emphasis on the different additives and processes that can have a direct impact on biocompatibility during and after 3D printing of polymer materials.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Droplet bioprinting of acellular and cell-laden structures at high-resolutions

Advances in digital light projection(DLP) based (bio) printers have made printing of intricate structures at high resolution possible using a wide range of photosensitive bioinks. A typical setup of a DLP bioprinter includes a vat or reservoir filled with liquid bioink, which presents challenges in terms of cost associated with bioink synthesis, high waste, and gravity-induced cell settling, contaminations, or variation in bioink viscosity during the printing process. Here, we report a vat-free, low-volume, waste-free droplet bioprinting method capable of rapidly printing 3D soft structures at high resolution using model bioinks and model cells. A multiphase many-body dissipative particle dynamics model was developed to simulate the dynamic process of droplet-based DLP printing and elucidate the roles of surface wettability and bioink viscosity. Process variables such as light intensity, photo-initiator concentration, and bioink formulations were optimized to print 3D soft structures (∼0.4–3 kPa) with a typical layer thickness of 50 µm, an XY resolution of 38 ± 1.5 μm and Z resolution of 237 ± 5.4 µm. To demonstrate its versatility, droplet bioprinting was used to print a range of acellular 3D structures such as a lattice cube, a Mayan pyramid, a heart-shaped structure, and a microfluidic chip with endothelialized channels. Droplet bioprinting, performed using model C3H/10T1/2 cells, exhibited high viability (90%) and cell spreading. Additionally, microfluidic devices with internal channel networks lined with endothelial cells showed robust monolayer formation while osteoblast-laden constructs showed mineral deposition upon osteogenic induction. Overall, droplet bioprinting could be a low-cost, no-waste, easy-to-use, method to make customized bioprinted constructs for a range of biomedical applications.

DLP↗
DOE OSTI2024

Shelf-Stable Bingham Plastic Polyurethane Thermosets for Additive Manufacturing

Here, this study presents an innovative 3D-printing method for fabricating hybrid-hardness polyurethane (PU) thermosets via direct-ink writing (DIW). This method features an unprecedentedly long pot-life of at least 16 months for uncured material, achieved by employing internally-blocked polymeric uredines as the isocyanate source. This innovation not only extends pot life but also broadens the pre-print processing temperature range. Surface-modified fumed silica, used as a rheology modifier, ensures the maintenance of Bingham fluid characteristics. Rigorous evaluations, including DSC, tensile tests, SEM, OM, and μ-CT, verify the material’s uniform and nearly isotropic structure, devoid of defects. DMA analysis reveals that these 3D-printed PUs withstand processing temperatures up to 240°C. The practical application of this technology is demonstrated through the successful 3D printing of a shoe sole, showcasing the ability to incorporate regions of varying hardness, highlighting the versatile property customization of this method.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Characterization of radiation damage in 3D printed SiC

The SiC fuel matrix for advanced gas-cooled high temperature reactors as part of the Transformational Challenge Reactor program serves as the fuel particle container structure, a barrier to fission gas release, and a heat transfer medium. Its performance is particularly important because the fuel matrix must demonstrate good structural stability and thermal behaviors. An additive manufacturing methodology combining a binder jet 3D printing process with chemical vapor infiltration (CVI) for the production of SiC was recently developed. In this study, post irradiation examination by transmission electron microscopy shows that defect accumulation within the printed particles is very similar to other forms of high-purity SiC. However, damage accumulation was not directly observed in the CVI matrix because black spot damage and dislocation loops are difficult to image within the nanoscale highly faulted CVI matrix and because interstitial defects may rapidly annihilate at the stacking faults. Therefore, electron energy loss spectroscopy (EELS) analysis was used to analyze defect swelling in both the printed particles and the CVI matrix. The EELS analysis helped reveal that the radiation-induced swelling in the CVI matrix is similar to that of the printed SiC particles. This work shows that 3D printed SiC has behavior that is comparable to SiC processed by other means and that 3D printing could serve as a suitable processing technique for high-purity SiC for nuclear applications.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Printed graphene oxide-based membranes for gas separation and carbon capture

Graphene oxide (GO)-based separation membranes have demonstrated the great potential to separate molecules and ions by the interlayer spacing with tunable nano-sized channels. The scalable fabrication of GO-based gas separation membranes, however, remains challenging, although a few preparation approaches have been reported. Here in this work, we present for the first time that the co-solvent ink-jet printing, as a fast and scalable method, can be utilized for scalable GO-based gas separation membrane preparation. Large-area (>100 cm 2 ), ultrathin, and high-quality GO membrane was successfully deposited on commercial polysulfone (PS) support, and characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and X-ray diffraction, et al., Selective hydrogen (H 2 ) and helium (He) transport over carbon dioxide (CO 2 ) and nitrogen (N 2 ) was demonstrated for the printed GO membrane. To further explore the separation potential of the printed GO-based gas membrane, additives for facilitated molecular transport were incorporated during the membrane printing process. By inserting CO 2 -philic agents into the printed GO membrane, highly efficient separation of CO 2 from N 2 was achieved with CO 2 /N 2 selectivity of 70 and CO 2 permeance as high as 2,500 GPU. The strategy proposed here may provide guidance for large-scale GO-based gas separation membrane production and a versatile approach for applying other functional 2-dimensional materials towards the membrane separation application.

42 ENGINEERING↗
DOE OSTI2022

The Electrochemical Behavior of As-Prepared Aluminum Alloy A360 Produced by Selective Laser Melting Fabrication with and without a Trivalent Chromium Process Conversion Coating

In this paper, we report on the electrochemical behavior and corrosion resistance of as-prepared aluminum alloy, A360 (AlSi10Mg), fabricated by additive manufacturing, with and without a trivalent chromium process conversion coating. Selective laser melting was the 3D printing process used for the alloy build. The corrosion suppression provided by the coating system was assessed through electrochemical measurements and accelerated degradation testing during a 14-day continuous neutral salt-spray exposure. The results indicate that the conversion coating can be formed by solution pretreating (degreasing and deoxidation) the alloy (X-Z plane perpendicular to the build plane) with its native surface roughness (as-prepared) followed by immersion for 10, 15 or 20 min in the coating bath. All three immersion times provide an equivalent level of corrosion protection to the alloy. The conversion coating suppresses both anodic and cathodic currents, increases the polarization resistance, and provides both anodic and cathodic corrosion protection to the as-prepared alloy. The conversion-coated specimens exhibit good stand-alone corrosion resistance during a 14-day neutral salt-spray exposure with corrosion intensity values (g/m 2 -year) ~10x lower than values for the uncoated, as-prepared alloy specimens.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Melt Pool characteristics on surface roughness and printability of 316L stainless steel in laser powder bed fusion

Purpose Surface quality and porosity significantly influence the structural and functional properties of the final product. This study aims to establish and explain the underlying relationships among processing parameters, top surface roughness and porosity level in additively manufactured 316L stainless steel. Design/methodology/approach A systematic variation of printing process parameters was conducted to print cubic samples based on laser power, speed and their combinations of energy density. Melt pool morphologies and dimensions, surface roughness quantified by arithmetic mean height (Sa) and porosity levels were characterized via optical confocal microscopy. Findings The study reveals that the laser power required to achieve optimal top surface quality increases with the volumetric energy density (VED) levels. A smooth top surface (Sa < 15 µm) or a rough surface with humps at high VEDs (VED > 133.3 J/mm 3 ) can serve as indicators for fully dense bulk samples, while rough top surfaces resulting from melt pool discontinuity correlate with high porosity levels. Under insufficient VED, melt pool discontinuity dominates the top surface. At high VEDs, surface quality improves with increased power as mitigation of melt pool discontinuity, followed by the deterioration with hump formation. Originality/value This study reveals and summarizes the formation mechanism of dominant features on top surface features and offers a potential method to predict the porosity by observing the top surface features with consideration of processing conditions.

Engineering↗
DOE OSTI2025

Design, fabrication, simulation, and testing of additively manufactured lattice-based copper heat sinks

Here, this study investigates the potential advantages of lattice structure-based bound metal material extrusion (MEX) 3D printing for fabricating high-performance copper heat sinks. Copper powder-filled polymer filaments, with a copper content of > 90 wt.%, were developed specifically for the bound metal MEX 3D printing process. Three types of structures—planar, strut, and surface lattices—were 3D printed to facilitate efficient heat transfer pathways within the heat sinks. Subsequent post-processing steps, including polymer removal and sintering, were performed to achieve dense copper parts. Hot isostatic pressing was further employed to enhance the sintered density from 93 to 98%. Finite element analysis (FEA) simulations were conducted to assess the heat transfer efficiency of the designs, and heat transfer experiments were performed using a custom setup to validate the simulation results. Additionally, this research explores the use of extended hold times during pre-sintering and a reduced atmosphere to enhance the %IACS values (electrical conductivity) and thermal performance of the bound metal MEX 3D printed copper heat sinks. The investigation combines experimental analysis, including simulations and heat transfer experiments, to gain insights into the structure-material property relationships and optimize the thermal performance of the printed heat sinks.

Ajjarapu, Kameswara Pavan Kumar [Oak Ridge Nationa↗
DOE OSTI2020

4D Printing via an Unconventional Fused Deposition Modeling Route to High-Performance Thermosets

An unprecedented four-dimensional (4D) printing process allowing high-performance and shape memory thermoset to be printed, for the first time, by fused deposition modeling (FDM) with isotropic properties has been achieved. Here, bisphenol A-based epoxy and benzoxazine were formulated to a low-temperature thermoplastic and high-temperature thermoset resin, which is melt-extrudable and can be postcured into covalently cross-linked material. Carbon nanotube (CNT) was added in the resin to work as both mechanical enhancement filler and rheology modifier to prevent shape deformation during postcuring process. The cross-layer reaction fuses individual layers into an integrity, thus eliminating layer delamination induced by FDM, offering isotropic mechanical properties regardless of the printing orientations. The highly cross-linked network provides outstanding mechanical strength and superb thermal stability. The excellent shape memory performance with fast recovery rate and large recovery degree is also obtained in the three-dimensional (3D) printed composites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Multiscale embedded printing of engineered human tissue and organ equivalents

Creating tissue and organ equivalents with intricate architectures and multiscale functional feature sizes is the first step toward the reconstruction of transplantable human tissues and organs. Existing embedded ink writing approaches are limited by achievable feature sizes ranging from hundreds of microns to tens of millimeters, which hinders their ability to accurately duplicate structures found in various human tissues and organs. In this study, a multiscale embedded printing (MSEP) strategy is developed, in which a stimuli-responsive yield-stress fluid is applied to facilitate the printing process. A dynamic layer height control method is developed to print the cornea with a smooth surface on the order of microns, which can effectively overcome the layered morphology in conventional extrusion-based three-dimensional bioprinting methods. Since the support bath is sensitive to temperature change, it can be easily removed after printing by tuning the ambient temperature, which facilitates the fabrication of human eyeballs with optic nerves and aortic heart valves with overhanging leaflets on the order of a few millimeters. The thermosensitivity of the support bath also enables the reconstruction of the full-scale human heart on the order of tens of centimeters by on-demand adding support bath materials during printing. Here, the proposed MSEP demonstrates broader printable functional feature sizes ranging from microns to centimeters, providing a viable and reliable technical solution for tissue and organ printing in the future.

3D bioprinting↗