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At least 37 records · Page 2

Gamma Radiation Aging Study of a Dow Corning SE 1700 Porous Structure Made by Direct Ink Writing

Dow Corning SE 1700 (reinforced polydimethylsiloxane) porous structures were made by direct ink writing (DIW). The specimens (~50% porosity) were subjected to a compressive strain of ~25% while exposed to a gamma radiation dose of 1, 5, or 10 Mrad under vacuum. Compression set and load retention of the aged specimens were measured after a ~24 h relaxation period. Compression set (relative to deflection) increased with radiation dose: 11, 35, and 51% after 1, 5, and 10 Mrad, respectively. Load retention was 96-97% for the doses tested. The SE 1700 compared favorably to M9763 cellular silicone tested under the same conditions.

36 MATERIALS SCIENCE↗

Gigahertz Electromagnetic Structures via Direct Ink Writing for Radio-Frequency Oscillator and Transmitter Applications

Radio–frequency (RF) electronics, which combine passive electromagnetic devices and active transistors to generate and process gigahertz (GHz) signals, provide a critical basis of ever–pervasive wireless networks. While transistors are best realized by top–down fabrication, relatively larger electromagnetic passives are within the reach of printing techniques. Here, direct writing of viscoelastic silver–nanoparticle inks is used to produce a broad array of RF passives operating up to 45 GHz. These include lumped devices such as inductors and capacitors, and wave–based devices such as transmission lines, their resonant networks, and antennas. Moreover, to demonstrate the utility of these printed RF passive structures in active RF electronic circuits, they are combined with discrete transistors to fabricate GHz self–sustained oscillators and synchronized oscillator arrays that provide RF references, and wireless transmitters clocked by the oscillators. Furthermore, this work demonstrates the synergy of direct ink writing and RF electronics for wireless applications.

36 MATERIALS SCIENCE↗

On the direct ink write (DIW) 3D printing of styrene-butadiene rubber (SBR)-based adhesive sealant

Direct Ink Writing (DIW) utilizes a wide range of ink formulations to produce desirable 3D-printed structures and properties. Styrene-butadiene rubber (SBR) is an attractive candidate for 3D printing owing to its commercial availability, rheology, excellent mechanical properties, good impact resilience, and chemical stability. The SBR-based sealant was 3D printed in a DIW process, even in an ambient environment. The rheological behavior was assessed and correlated with optimized printing parameters. Important physico-chemical properties of the 3D-printed material were reported showing excellent properties as an elastomer. Finally, this work should expand the potential applications of existing rubber-based materials in additive manufacturing.

36 MATERIALS SCIENCE↗

Three-dimensional hierarchical nanoporous copper via direct ink writing and dealloying

Three-dimensional (3D) hierarchical nanoporous Cu (3DHNP-Cu) is synthesized using a combination of direct ink writing (DIW) based 3D printing, thermal sintering, and chemical dealloying of Mn–Cu alloys. Through tuning processing conditions such as ink composition and cooling rate (after sintering), with consideration of Mn loss during sintering, 3DHNP-Cu with fully bicontinuous nanostructures and negligible residual Mn can be produced after dealloying. The 3DHNP-Cu is comprised of structural features that span seven orders of magnitude, where DIW digitally controls macroscale porous features, thermal sintering and degradation of the binding polymer determines microscale porous features, and dealloying gives rise to nanoscale pores.

36 MATERIALS SCIENCE↗

Universal Design Curves for Elastomeric Direct Ink-Writing Architectures

Direct ink writing of silicone elastomers enables printing with precise control of porosity and mechan- ical properties of ordered cellular solids, suitable for shock absorption and stress mitigation applications. With the ability to manipulate structure and feedstock stiffness, the design space becomes challenging to parse to obtain a solution producing a desired mechanical response. Here we derive an analytical design approach for a specific architecture. Results from finite element simulations and quasi-static mechanical tests of two different parallel strand architectures were analyzed to understand the structure-property relationships under compressive strain. Combining effective stiffness-density scaling with least squares optimization of the stress responses yielded general response curves parameterized by resin modulus and strand spacing. An analytical expression of these curves serves as a reduced order model, which, when optimized, provides a rapid design capability for filament-based 3D printed structures. As a demonstration, the optimal design of a face-centered tetragonal architecture is computed that satisfies prescribed minimum and maximum load constraints.

36 MATERIALS SCIENCE↗

One-Component, Vinyl-Functional Fluorosilicone Pastes for Direct Ink Write Additive Manufacturing

In this study, one-component (“all-in-one”) fluorosilicone pastes specifically designed for application in direct ink write (DIW) additive manufacturing (AM) have been developed. They consist of vinyl-functional, methyltrifluoropropyl-containing (MeTfpS) terpolysiloxane base polymer(s), hydrosilyl-functional cross-linker(s), UV-sensitive hydrosilylation catalyst, thixotropic additive, and trimethylsilylated fumed silica filler, with other additives that are optional. Their base polymers were completely amorphous and linear, with molecular weights (M n ) ranging from approximately 7000 to 50,000 and specifically targeted for the viscosity range ideal for DIW. These polymers were prepared by anionic ring-opening polymerizations (A-ROP) of appropriate mixtures of cyclic siloxanes initiated by oligomeric, difunctional tetramethylammonium silanolate in the presence of a difunctional tetramethyldivinyldisiloxane end-blocker and molecular weight regulator. Two series of these terpolymers were prepared: one containing 5 mol % MeTfpS repeat units but varying degrees of polymerization (DP) from 80 to 600 and the other containing 5, 10, and 15 mol % MeTfpS at a constant DP of 600. All polymers contained mostly random distributions of MeTfpS repeat units. The pastes were prepared by speed-mixing, ready for use in DIW, they exhibited ideal thixotropy, long-term (over a year) rheological stability, and can be quickly (within seconds) and permanently cured by room-temperature, UV-activated hydrosilylation in air. The resulting elastomers showed base polymer molecular weight- and composition-dependent stress-induced crystallization (SIC) at higher molecular weights and lower trifluoropropyl contents and tunable Shore A hardness (30A–40A) typical for soft polysiloxane rubbers. Preliminary DIW tests indicated excellent printability with high precision of printed shapes and clearly present these one-component pastes as prime candidates for simple and practical printing of silicone elastomer objects.

36 MATERIALS SCIENCE↗

Towards gradient multimaterial toolpath generation for direct ink writing with connected fermat spirals

This work describes advances towards a reproducible, parametrically defined algorithm for generating graded multimaterial toolpaths for direct ink writing. Expanding on the existing Fermat space-filling algorithm and coupling with image-driven processing techniques, we demonstrate the fabrication of multimaterial structures. Here, material composition is encoded within toolpaths by parsing hue values from a multi-colored image. By performing dynamic velocity compensation based on local curvature and Euclidean distance filtering, internal voids are mitigated while optimizing print fidelity. Here, the work opens new avenues for designing complex toolpaths with locally programmable composition.

3D Printing↗

PDMS ‐silica composite gas separation membranes by direct ink writing

Abstract Polydimethylsiloxane (PDMS)‐based membranes containing amine‐functionalized and unfunctionalized silica particles were fabricated via direct ink writing for CO 2 /N 2 gas separation. The printability of the inks was evaluated by rheological measurements, while spectroscopy, microscopy, thermal measurements, and mechanical testing were employed to characterize the printed membranes. The surface morphology of the membranes revealed the absence of voids, demonstrating their suitability for gas separation. The printed membranes also exhibited desirable thermal and mechanical properties (i.e., thermal degradation temperature of 518 °C and tensile strength as high as 1.178 MPa with 529% elongation). The PDMS‐based membranes generally displayed high permeability for CO 2 but slightly low selectivity for the CO 2 /N 2 gas pair. The best‐combined permeability‐selectivity performance of 8794 barrer and selectivity of 11.64 was demonstrated by the printed PDMS membrane containing no SiO 2 fillers. The inclusion of unfunctionalized SiO 2 particles generally increased the membrane's gas permeability but compromised the selectivity. In contrast, membranes with amine‐functionalized silica showed improved selectivity compared to membranes containing unfunctionalized silica. Overall, the performance and characteristics offered by the PDMS/silica composite membranes demonstrated the potential of 3D printing as an economical and sustainable fabrication approach to developing materials for carbon capture applications.

Gutierrez, Dianne B.↗

On the cogent formulation of an elastomeric silicone ink material for direct ink write ( DIW ) 3D printing

Abstract Adhesives and sealants show fine rheology with good physical and mechanical properties as viscous pastes, a possible starting point for developing direct ink writing (DIW) 3D printing ink. However, many commercial adhesives and sealants take days or weeks to cure fully. DIW 3D‐printed parts made directly from these sealants are not designed for a scalable manufacturing process and high‐volume production. Moreover, most of these adhesives and sealants have volume shrinkage during cure. A systematic understanding of formulation methods and design principles for an elastomeric silicone DIW ink can overcome these issues. This study presents the cogent formulation development of a 3D printable thermoset elastomer silicone that gels and cures isotropically in minutes, reducing cycle time for rapid ink development with no shrinkage during cure. More specifically, we outline the principles of raw material selection of a formulation to achieve excellent rheology, printability, synchronized working, and gel time fitting requirements closer to scalable manufacturing. The reaction kinetics and their corresponding 3D‐printed structural properties are also described. Interest in future work is toward a rational DIW 3D printing ink material development protocol and use of machine learning (ML). Highlights Formulation method flexibility and design principle of DIW ink. Raw material selection principle to achieve optimal rheology for DIW printing. Ink gel kinetics for large‐scale DIW manufacturing. Hydrosilylation conversion over time at different ambient temperatures. Structural properties of DIW 3D printed parts.

36 MATERIALS SCIENCE↗

Load Deflection of Dow Corning SE 1700 Face Centered Tetragonal Direct Ink Write Materials: Effect of Thickness and Filament Spacing

Dow Corning SE 1700 (reinforced polydimethylsiloxane) porous structures were made by direct ink writing (DIW) in a face centered tetragonal (FCT) configuration. The filament diameter was 250 μm. Structures consisting of 4, 8, or 12 layers were fabricated with center-to-center filament spacing (“road width” (RW)) of 475, 500, 525, 550, or 575 μm. Three compressive load-unload cycles to 2000 kPa were performed on four separate areas of each sample; three samples of each thickness and filament spacing were tested. At a given strain during the third loading phase, stress varied inversely with porosity. At 10% strain, the stress was nearly independent of the number of layers (i.e., thickness). At higher strains (20- 40%), the stress was highest for the 4-layer structure; the 8- and 12-layer structures were nearly equivalent suggesting that the load deflection is independent of number of layers above 8 layers. Intra-and inter-sample variability of the load deflection response was higher for thinner and less porous structures.

36 MATERIALS SCIENCE↗

Load Deflection of Dow Corning SE 1700 Simple Cubic Direct Ink Write Materials: Effect of Thickness and Filament Spacing

Dow Corning SE 1700 (reinforced polydimethylsiloxane) porous structures were made by direct ink writing (DIW) in a simple cubic (SC) configuration. The filament diameter was 250 μm. Structures consisting of 4, 8, or 12 layers were fabricated with center-to-center filament spacing (“road width” (RW)) of 475, 500, 525, 550, or 575 μm. Three compressive load-unload cycles to 2000 kPa were performed on four separate areas of each sample; three samples of each thickness and filament spacing were tested. Geometry-dependent buckling of the SC structure was evident. At a given strain during the third loading phase, stress varied inversely with porosity. At strains of 25% and higher, the stress varied inversely with the number of layers (i.e., thickness); however, the relationship between stress and number of layers was more complex at lower strains. Intra-and inter-sample variability of the load deflection response was higher for thinner and less porous structures.

36 MATERIALS SCIENCE↗

Thermal Aging Study of a Dow Corning SE 1700 Porous Structure Made by Direct Ink Writing: 1-Year Results and Long-Term Predictions

Dow Corning SE 1700 (reinforced polydimethylsiloxane) porous structures were made by direct ink writing (DIW). The specimens (~50% porosity) were subjected to various compressive strains (15, 30, 45%) and temperatures (room temperature, 35, 50, 70°C) in a nitrogen atmosphere (active purge) for 1 year. Compression set and load retention of the aged specimens were measured periodically during the study. Compression set increased with strain and temperature. After 1 year, specimens aged at room temperature, 35, and 50°C showed ~10% compression set (relative to the applied compressive deflection), while those aged at 70°C showed 20-40%. Due to the increasing compression set, load retention decreased with temperature, ranging from ~90% at room temperature to ~60-80% at 70°C. Long-term compression set and load retention at room temperature were predicted by applying time-temperature superposition (TTS). The predictions show compression set relative to the compressive deflection will be ~10-15% with ~70-90% load retention after 50 years at 15-45% strain, suggesting the material will continue to be mechanically functional. Comparison of the results to previously acquired data for cellular (M97*, M9760, M9763) and RTV (S5370) silicone foams suggests that the SE 1700 DIW porous specimens are on par with, or outperform, the legacy foams.

36 MATERIALS SCIENCE↗

Coaxial Direct Ink Writing of Cholesteric Liquid Crystal Elastomers in 3D Architectures

Abstract Cholesteric liquid crystal elastomers (CLCEs) hold great promise for mechanochromic applications in anti‐counterfeiting, smart textiles, and soft robotics, thanks to the structural color and elasticity. While CLCEs are printed via direct ink writing (DIW) to fabricate free‐standing films, complex 3D structures are not fabricated due to the opposing rheological properties necessary for cholesteric alignment and multilayer stacking. Here, 3D CLCE structures are realized by utilizing coaxial DIW to print a CLC ink within a silicone ink. By tailoring the ink compositions, and thus, the rheological properties, the cholesteric phase rapidly forms without an annealing step, while the silicone shell provides encapsulation and support to the CLCE core, allowing for layer‐by‐layer printing of self‐supported 3D structures. As a demonstration, free‐standing bistable thin‐shell domes are printed. Color changes due to compressive and tensile stresses can be witnessed from the top and bottom of the inverted domes, respectively. When the domes are arranged in an array and inverted, they can snap back to their base state by uniaxial stretching, thereby functioning as mechanical sensors with memory. The additive manufacturing platform enables the rapid fabrication of 3D mechanochromic sensors thereby expanding the realm of potential applications for CLCEs.

36 MATERIALS SCIENCE↗

Direct ink write multi-material printing of PDMS-BTO composites with MWCNT electrodes for flexible force sensors

Here, with recent advances of additive manufacturing technology, direct ink write (DIW) printing has allowed to incorporate multi-material printing of various materials with freedom of design and complex geometric shapes to complete functional sensors in a one-step fabrication. This paper introduces the use of DIW 3D printing of polydimethylsiloxane (PDMS) with barium titanate (BTO) filler as stretchable composites with tunable piezoelectric properties that can be used for force sensors applications. To improve the bonding between stretchable piezoelectric composites and electrodes, multi-walled carbon nanotubes was included in the fabrication of electrodes at a fixed ratio of 11 wt. %. The alignment of the BTO dipoles was achieved through corona poling method, which applies an electric charge on the surface layer of the functional material, aligning the dipoles in the desired direction and thus gaining the piezoelectricity. Different BTO mixing ratios (10–50 wt. %) were evaluated in order to obtain tunable piezoelectric properties and compare the sensitivity with respect their elastic properties. Tensile testing and piezoelectric testing were carried out to characterize mechanical and piezoelectric properties. Results showed that fabricated PDMS with 50 wt. % BTO gave the highest piezoelectric coefficient (d 33 ) of 11.5 pC N -1 and with an output voltage of 385 mV under compression loading of >200 lbF. This demonstrates feasibility of using multi-material DIW printing to fabricate piezoelectric force sensors with integrated electrodes in one-step without compromising the flexibility of the material.

36 MATERIALS SCIENCE↗

Advanced Methods for Direct Ink Write Additive Manufacturing

Lawrence Livermore National Laboratory is one of the world’s premier labs for research and development of additive manufacturing processes. Out of these many processes, direct ink write (DIW) is arguably one of the most relevant for the manufacture of architected polymeric materials, components and hardware. However, a bottleneck in this pipeline that has largely been ignored to date is the lack of advanced software implementation with respect to toolpath execution. There remains to be a convenient, automated method to design and produce complex parts that is user-friendly and enabling for the realization of next generation designs and structures. For a material to be suitable as a DIW ink it must possess the appropriate rheological properties for this process. Most importantly, the material must exhibit shear-thinning in order to extrude through a print head and have a rapid recovery of its static shear modulus. This makes it possible for the extrudate to be self-supporting upon exiting the print head. While this and other prerequisites narrow the scope of ‘offthe- shelf’ printable materials directly amenable to DIW, the process still tolerates a wide range of potential feedstock materials. These include metallic alloys, inorganic solvent borne dispersions, polymeric melts, filler stabilized monomer compositions, pre-elastomeric feedstocks and thermoset resins each of which requires custom print conditions tailored to the individual ink. As such, an ink perfectly suited for DIW may be prematurely determined to be undesirable for the process if printed under the wrong conditions. Defining appropriate print conditions such as extrusion rate, layer height, and maximum bridge length is a vital first step in validating an ink’s DIW capability.

36 MATERIALS SCIENCE↗

Direct ink writing of aqueous-based Gadolinium (III) oxide slurries

Gadolinium (III) oxide (gadolinia, Gd 2 O 3 ) has recently been identified as an intriguing material for applications in the medical, solid oxide fuel cell, and nuclear industries. This interest drives the need for developing and understanding manufacturing techniques that can produce dense Gd 2 O 3 structures. Direct ink writing (DIW), an extrusion-based additive manufacturing method, has also garnered interest because of its capability to produce dense ceramic parts with increased complexity in an economical manner. In this study, DIW was explored as a manufacturing technique for Gd 2 O 3 . Experiments were performed to develop Gd 2 O 3 bearing inks capable of being processed via DIW. Ink solids loading and sintering temperatures were varied to assess their impact on the final density and microstructure. Optimum sintering conditions are proposed and were experimentally verified at a dwell temperature of 1500°C. Gd 2 O 3 samples were successfully manufactured using DIW, achieving densities greater than 96 % of the theoretical density.

36 MATERIALS SCIENCE↗

Direct Ink Write 3D Printing of Fully Dense and Functionally Graded Liquid Metal Elastomer Foams

Liquid metal (LM) elastomer composites offer promising potential in soft robotics, wearable electronics, and human-machine interfaces. Direct ink write (DIW) 3D printing offers a versatile manufacturing technique capable of precise control over LM microstructures, yet challenges such as interfilament void formation in multilayer structures impact material performance. Here, a DIW strategy is introduced to control both LM microstructure and material architecture. Investigating three key process parameters–nozzle height, extrusion rate, and nondimensionalized nozzle velocity–it is found that nozzle height and velocity predominantly influence filament geometry. The nozzle height primarily dictates the aspect ratio of the filament and the formation of voids. A threshold print height based on filament geometry is identified; below the height, significant surface roughness occurs, and above the ink fractures, which facilitates the creation of porous structures with tunable stiffness and programmable LM microstructure. These porous architectures exhibit reduced density and enhanced thermal conductivity compared to cast samples. When used as a dielectric in a soft capacitive sensor, they display high sensitivity (gauge factor = 9.0), as permittivity increases with compressive strain. These results demonstrate the capability to simultaneously manipulate LM microstructure and geometric architecture in LM elastomer composites through precise control of print parameters, while maintaining geometric fidelity in the printed design.

Spencer Pak↗