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At least 307 records · Page 17

3D printing of void-free glass monoliths: rheological and geometric considerations

Direct ink writing (DIW) is a versatile additive manufacturing technique capable of printing 3D architectures from a broad range of materials. The key advantage of DIW is the ability to spatially control both the architecture and the composition of the printed part, which enables the production of components with previously unachievable combinations of functionalities. One emergent application space for DIW has been in additively manufactured glass optics, where a “green body” is patterned layer-by-layer by extruding a silica-based slurry through a microfluidic nozzle and then thermally consolidated to transparent glass. A critical aspect of the process is ensuring that the printed part is completely free of voids that can occur in the interstitial spaces between the extruded filaments. This outcome is governed by the interplay between ink rheology and strains imposed by the printing process and geometric packing of the filaments. Here, we explore the strain- and rate-dependent deformation events in the DIW process to determine conditions that enable the printing of void-free monoliths without sacrificing shape fidelity. We focus on yield stress fluids consisting of fumed silica nanoparticles dispersed in organic solvents at varied volume fractions to control the rheological properties. We investigate the printability of these ink materials as a function of print process variables and devise the appropriate dimensionless parameters that capture the geometry-dependent and rate-dependent effects on the deformation of the extruded ink. Lastly, we use these scaling arguments to construct a phase diagram for void-free monolith printability.

36 MATERIALS SCIENCE↗

La–Sr–Co oxide catalysts for oxygen evolution reaction in anion exchange membrane water electrolyzer: The role of electrode fabrication on performance and durability

Anion exchange membrane water electrolysis is an attractive technology for low-cost generation of “green” hydrogen by combining the use of noble metal-free catalysts with pure water feed. By thus addressing main drawbacks of the liquid alkaline electrolysis and proton exchange membrane water electrolysis, anion exchange membrane water electrolysis stands an excellent chance of replacing the two technologies. The development of active and stable platinum group metal (PGM)-free catalysts for oxygen evolution reaction (OER) is crucial for making anion exchange membrane water electrolyzers (AEMWEs) practical. For this work, we synthesized, characterized and tested two La–Sr–Co oxide-based OER catalysts. First, we characterized the catalysts by XRD, SEM, and N 2 physisorption and assessed their OER activity in a three-electrode cell. Next, we focused on electrode fabrication, demonstrating the importance of catalyst-ink application to the porous transport layers (PTLs) and a key role of adding a binder to the catalyst ink to prevent the catalyst detachment from the PTL in pure water. We tested three membrane electrode assemblies prepared using different formulations of the anode catalyst ink. The results show that the optimum ink formulation is essential for the performance on pure-water feed by maximizing OH - conductivity of the catalyst layer and catalyst-membrane interface.

47 OTHER INSTRUMENTATION↗

Simulation of two nanoparticle melting to understand the conductivity drop of 3D-printed silver nanowires

The future flexible sensor technology will require low-temperature, fast processing 3D printing techniques that will rely heavily on the quality of nanoparticle (NP) Ink. Electrical conductivity has been found to decrease in majority of the 3D printed electronic wires. Herein we report a fundamental understanding in drop of electrical conductivity in processed silver (Ag) line wire, generally found in Ag-nanoparticle Ink, using large-scale atomistic molecular dynamics (MD) simulations of sintering of five different sizes of Ag NPs. To preserve the high conductivity of pure silver wires, the integrity of the pristine face-centered cubic (FCC) crystalline structure must be retained in the processed line wires. Simulations show that the pristine Ag FCC structures of the nanoparticles are not recovered after melting and resolidification, instead, the resolidified material is paracrystaline. The breakdown of pristine FCC structures might be the cause of the drop in conductivity of processed Ag wires. Simulation results suggest that the intermediate size nanoparticles retain highest percentage of the pristine silver face-centered cubic (FCC) structure after pulse treatments. Our results show that the most promising Ag-Ink should contain smaller to medium size silver NPs that can retain FCC structure after 3D printing of the Ag-Ink.

42 ENGINEERING↗

All 2D Material Printed Diodes and Circuits on Paper for Sustainable Electronics

Sustainable electronics aim to reduce environmental impact by using ecofriendly materials, energy-efficient manufacturing, and recyclable components. However, existing approaches rely on complex, resource-intensive methods, rare metals, or nanomaterials with limited stability as well as plastic substrates, raising sustainability issues. Solution-processed two-dimensional (2D) materials offer a promising alternative: water-based and biocompatible conductive, semiconductive, and insulating 2D material inks can be produced with scalable techniques and are suitable for the fabrication of fully printed devices on low-cost and biodegradable paper substrates. However, 2D material only and fully printed diodes on paper have not yet been reported. Here, we demonstrate fully inkjet-printed 2D material-based diodes on paper using metal-insulator-semiconductor and metal-insulator-metal-semiconductor architectures. Water-based graphene and MoS2 inks, prepared by liquid-phase exfoliation, are used for the metallic and insulating films, while electrochemical exfoliation is used to produce the semiconducting MoS2 ink. The highest forward-to-reverse current ratio obtained is 330 (at ±2 V), while the forward current density is 1 mA/cm2 (at 1 V), making the diode performance comparable to the best solution-processed diodes reported so far. However, in contrast to previous works, fabrication occurs entirely at room temperature and ambient pressure, without using high-pressure sputtering, thermal evaporation, and any precious metal ink. The devices maintain stable performance under bending up to strain of 4% over 10,000 cycles. Finally, the diodes are successfully integrated with other 2D-material based electrical components to realize fully printed RC circuits, differentiators, integrators, and AC-to-DC converters onto paper, hence demonstrating the suitability of our approach for sustainable and disposable integrated circuits.

2D materials↗

Spatially programmed alignment and actuation in printed liquid crystal elastomers

Liquid crystal elastomers (LCEs) exhibit reversible shape morphing behavior when cycled above their nematic-to-isotropic transition temperature. During extrusion-based 3D printing, LCE inks are subjected to coupled shear and extensional flows that can be harnessed to spatially control the alignment of their nematic director along prescribed print paths. Here, we combine experiment and modeling to elucidate the effects of ink composition, nozzle geometry, and printing parameters on director alignment. From rheological measurements, we quantify the dimensionless Weissenberg number ( Wi ) for the flow field each ink experiences as a function of printing conditions and demonstrate that Wi is a strong predictor of LCE alignment. We find that director alignment in LCE filaments printed through a tapered nozzle varies radially when Wi < 1, while it is uniform when Wi ≫ 1. Based on COMSOL simulations and in operando X-ray measurements, we show that LCE inks printed through nozzles with an internal hyperbolic geometry exhibit a more uniform director alignment for a given Wi compared to those through tapered nozzles. Concomitantly, the stiffness along the print direction and actuation strain of printed LCEs increases substantially under such conditions. By varying Wi during printing through adjusting the flow rate “on the fly”, LCE architectures with uniform composition, yet locally encoded shape morphing transitions can be realized.

36 MATERIALS SCIENCE↗

Understanding and mitigating process drift in aerosol jet printing

Aerosol jet printing offers a versatile, high-resolution prototyping capability for flexible and hybrid electronics. Despite its rapid growth in recent years, persistent problems such as process drift hinder the adoption of this technology in production environments. Here we explore underlying causes of process drift during aerosol jet printing and introduce an engineered solution to improve deposition stability. In this work it is shown that the ink level within the cartridge is a critical factor in determining atomization efficiency, such that the reduction in ink volume resulting from printing itself can induce significant and systematic process drift. By integrating a custom 3D-printed cartridge with an ink recirculation system, ink composition and level within the cartridge are better maintained. This strategy allows extended duration printing with improved stability, as evidenced by 30 h of printing over 5 production runs. This provides an important tool for extending the duration and improving reliability for aerosol jet printing, a key factor for integration in practical manufacturing operations.

36 MATERIALS SCIENCE↗

FY2020 Annual Report on Subcontract B631779 with UC Berkeley: Reactive Precursors Additive Manufacturing Report

This work succeeded in reaching each of the stated milestones for developing, printing, reacting, and characterizing the uranium carbide final products. Leveraging experience gained from creating magnesium oxide inks (milestone #1) and prior reactive precursor work with boron carbide (milestone #2) a uranium carbide reactive precursor ink was developed. The chosen composition of ink utilized a mixture of wax, petrolatum, and stearic acid as the binder. The reactive precursor portion of the ink was comprised of uranium oxide and nano particle activated carbon for production of uranium carbide via carbothermal reduction. Following an in-air burnout of the binder at 160C the printed samples were reacted and sintered at 1750C in an argon environment induction furnace. The resulting product has an open porosity dense, foam-like internal structure with a calculated density of 89% in the solid fraction.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Scalable Approaches to Address Thermomechanical and Chemical Instabilities in Metal Halide Perovskites

We will discuss our group’s recent efforts to address the thermomechanical and chemical instabilities of metal halide perovskites through multiple approaches. These approaches cover several length scales and aim to provide better understanding of behavior in all stages of processing—i.e., precursor behavior in inks, growth behavior of films during printing, and resulting optoelectronic properties and robustness of perovskite films and devices. We will highlight our efforts toward scalable printing of high-quality perovskite using the method recently invented by our group restricted area printing by ink drawing (RAPID). Additionally, we will discuss how molecular additives in precursor inks can influence the stability of the inks and resultant films. Finally, we will also describe our recent progress in addressing the poor mechanical toughness of perovskite using multifunctional nanofiber reinforcements. Together, all of these concepts are complimentary and compatible with scalable printing of perovskites and a necessary step towards developing a viable technology with long operational lifetimes.

Printz, Adam↗

MOD silver metallization for photovoltaics

The feasibility of utilizing metallo-organic decomposition (MOD) silver inks were investigated for front contact metallization of solar cells. Generic synthesis procedures were developed for all metallo-organic compounds investigated. Silver neodecanoate was found to be the most suitable silver metallo-organic compound for use in thick film inks, but the quality of the inks was found to be highly dependent on its purity. Although neither the process nor inks were completely optimized for solar cell front contact metallization, they show great promise for this application.

Vest, G. M.↗

Power assist EVA glove development

Structural modeling of the EVA glove indicates that flexibility in the metacarpophalangeal (MCP) joint can be improved by selectively lowering the elasticity of the glove fabric. Two strategies are used to accomplish this. One method uses coil springs on the back of the glove to carry the tension in the glove skin due to pressurization. These springs carry the loads normally borne by the glove fabric, but are more easily deformed. An active system was also designed for the same purpose and uses gas filled bladders attached to the back of the EVA glove that change the dimensions of the back of the glove and allow the glove to bend at the MCP joint, thus providing greater flexibility at this joint. A threshold control scheme was devised to control the action of the joint actuators. Input to the controller was provided by thin resistive pressure sensors placed between the hand and the pressurized glove. The pressure sensors consist of a layer of polyester film that has a thin layer of ink screened on the surface. The resistivity of the ink is pressure dependent, so an extremely thin pressure sensor can be fabricated by covering the ink patch with another layer of polyester film and measuring the changing resistance of the ink with a bridge circuit. In order to sense the force between the hand and the glove at the MCP joint, a sensor was placed on the palmar face of the middle finger. The resultant signal was used by the controller to decide whether to fill or exhaust the bladder actuators on the back of the glove. The information from the sensor can also be used to evaluate the effectiveness of a given control scheme or glove design since the magnitude of the measured pressures gives some idea of the torque required to bend a glove finger at the MCP joint. Tests of this actuator, sensor, and control system were conducted in an 57.2 kPa glove box by performing a series of 90 degree finger bends with a glove without an MCP joint assembly, a glove with the coil spring assembly, and with the four fingered actuated glove. The tests of these three glove designs confirm the validity of the model.

Main, John A.↗

JOVE Pilot Research Study in Astronomy and Microgravity Sciences

The purpose of this project was to develop hardware and software facilities for evaluating the biomechanical interactions between human hands and space suit gloves. We have constructed a prototype of the glove to demonstrate its sensing technologies. There are two types of sensors in the glove. The positions of the fingers are measured using bend sensors based on the CyberGlove design. This sensor consists of two strain gages mounted to a 0.003 inch thick mylar sheet. The sensor is encapsulated using 0.001 inch kapton film to give it sufficient rigidity. A long gage is used to average the strain generated in the sensor due to bending. This average strain produces an output signal proportional to the angle of the bend. The force sensor, FSR, is manufactured by Interlink. It consists of conductive ink sandwiched between two plastic sheets. An electrode is printed on one of the plastic sheets using silver ink. When the electrode makes contact, current flows through the conductive ink. The resistance of the ink pad is sensitive to pressure. We have also developed circuits for exciting and measuring the sensors. The current version requires a single sided twelve volt power supply which is one inch long and 0.4 inches in diameter.

Strauss, Alvin M.↗

Fully Printed, Flexible, Phased Array Antenna for Lunar Surface Communication

NASAs future exploration missions focus on the manned exploration of the Moon, Mars, and beyond, which will rely heavily on the development of a reliable communications infrastructure from planetary surface-to-surface, surface-to-orbit, and back to Earth. Flexible antennas are highly desired in many scenarios. Active phased array antennas (active PAAs) with distributed control and processing electronics at the surface of an antenna aperture offer numerous advantages for radar communications. Large-area active PAAs on flexible substrates are of particular interest in NASA s space radars due to their efficient inflatable package that can be rolled up during transportation and deployed in space. Such an inflatable package significantly reduces stowage volume and mass. Because of these performance and packaging advantages, large-area inflatable active PAAs are highly desired in NASA s surface-to-orbit and surface-to-relay communications. To address the issues of flexible electronics, a room-temperature printing process of active phased-array antennas on a flexible Kapton substrate was developed. Field effect transistors (FETs) based on carbon nanotubes (CNTs), with many unique physical properties, were successfully proved feasible for the PAA system. This innovation is a new type of fully inkjet-printable, two-dimensional, high-frequency PAA on a flexible substrate at room temperature. The designed electronic circuit components, such as the FET switches in the phase shifter, metal interconnection lines, microstrip transmission lines, etc., are all printed using a special inkjet printer. Using the developed technology, entire 1x4, 2x2, and 4x4 PAA systems were developed, packaged, and demonstrated at 5.3 GHz. Several key solutions are addressed in this work to solve the fabrication issues. The source/drain contact is developed using droplets of silver ink printed on the source/drain areas prior to applying CNT thin-film. The wet silver ink droplets allow the silver to wet the CNT thin-film area and enable good contact with the source and drain contact after annealing. A passivation layer to protect the device channel is developed by bonding a thin Kapton film on top of the device channel. This film is also used as the media for transferring the aligned CNT thin-film on the device substrate. A simple and cost-effective technique to form multilayer metal interconnections on flexible substrate is developed and demonstrated. Contact vias are formed on the second substrate prior to bonding on the first substrate. Inkjet printing is used to fill the silver ink into the via structure. The printed silver ink penetrates through the vias to contact with the contact pads on the bottom layer. It is then annealed to form a good connection. One-dimensional and two-dimensional PAAs were fabricated and characterized. In these circuits, multilayer metal interconnects were used to make a complete PAA system.

Subbaraman, Harish↗

Solid-State Ultracapacitor for Improved Energy Storage

NASA's Marshall Space Flight Center has developed a solid-state ultracapacitor using a novel nanocomposite, dielectric material. The material's design is based on the internal barrier layer capacitance (IBLC) concept, and it uses novel dielectric and metallic conductive ink formulations. Novel processing methods developed by NASA provide for unique dielectric properties at the grain level. Nanoscale raw material powders are tailored using a variety of techniques and then formulated into a special ink. This dielectric ink is used with novel metallic conductive ink to print a capacitor layer structure into any design necessary to meet a range of technical requirements. The innovation is intended to replace current range safety batteries that NASA uses to power the systems that destroy off-course space vehicles. A solid-state design provides the needed robustness and safety for this demanding application.

Nabors, Sammy↗

Solid State Ultracapacitor

An ink of the formula: 60-80% by weight BaTiO3 particles coated with SiO2; 5-50% by weight high dielectric constant glass; 0.1-5% by weight surfactant; 5-25% by weight solvent; and 5-25% weight organic vehicle. Also a method of manufacturing a capacitor comprising the steps of: heating particles of BaTiO3 for a special heating cycle, under a mixture of 70-96% by volume N2 and 4-30% by volume H2 gas; depositing a film of SiO2 over the particles; mechanically separating the particles; incorporating them into the above described ink formulation; depositing the ink on a substrate; and heating at 850-900 C for less than 5 minutes and allowing the ink and substrate to cool to ambient in N2 atmosphere. Also a dielectric made by: heating particles of BaTiO3 for a special heating cycle, under a mixture of 70-96% by volume N2 and 4-30% by volume H2 gas; depositing a film of SiO2 over the particles; mechanically separating the particles; forming them into a layer; and heating at 850-900 C for less than 5 minutes and allowing the layer to cool to ambient in N2 atmosphere.

Rolin, Terry D.↗

Impact of Synthesis and Aging on Titanium Carbide MXenes for Printed Microsystems

This work investigates the long-term electrical stability of Ti3C2Tx MXene Inks under accelerated aging conditions. Inks were synthesized from commercial MAX-Phase precursors, drop-cast onto custom PCB’s and monitored automated in-situ measurements. Samples aged at 85°C/85% RH, 85°C/0% RH and ambient conditions revealed distinct degradation trends. Wet aged inks showed rapid resistance increased while etched formulations exhibited long term stability. These findings highlight the influence of synthesis stage and environmental exposure on MXene Inks reliability, offering critical insights for printed MEMS and sensor applications. Ongoing measurements extend the aging timeline beyond prior studies, marking the longest evaluation under accelerated aging conditions to date.

Aging↗

Approaching the Practical Conductivity Limits of Aerosol Jet Printed Silver

Previous efforts to directly write conductive metals have been narrowly focused on nanoparticle ink suspensions that require aggressive sintering (>200°C) and result in low-density, small-grained agglomerates with electrical conductivities <25% of bulk metal. Here, we demonstrate aerosol jet printing of a reactive ink solution and characterize high-density (93%) printed silver traces having near-bulk conductivity and grain sizes greater than the electron mean free path, while only requiring low temperature (80°C) treatment. We have developed a predictive electronic transport model which correlates the microstructure to the measured conductivity and identifies a strategy to approach the practical conductivity limit for printed metals. Our analysis of how grain boundaries and tortuosity contribute to electrical resistivity provides insight into the basic materials science that governs how an ink formulator or process developer might approach improving the conductivity. Transmission line measurements validate that electrical properties are preserved up to 20GHz, which demonstrates the utility of this technique for printed RF components. Finally, this work reveals a new method of producing robust printed electronics that retain the advantages of rapid prototyping and three-dimensional fabrication while achieving the performance necessary for success within the aerospace and communications industries.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Refractive Index and Abbe Number Tuning via 3D Printable Optical Quality Silica–Titania–Germania Glasses

The development of optical quality GeO 2 –TiO 2 –SiO 2 glasses compatible with direct ink writing (DIW) 3D printing is reported in this study. Colloidal GeO 2 and TiO 2 –SiO 2 core–shell feedstocks are prepared by a sol–gel method and converted to printable inks for DIW. Printed inks are subsequently densified to glass using heat treatment at temperatures up to 1100 °C in air. A series of print‐compatible glass compositions are prepared, yielding transparent glass with the highest refractive index n = 1.576. Herein, it is shown that more TiO 2 can be incorporated into the glass without haziness or scattering through the addition of GeO 2 . The mechanisms for this are discussed, and it is shown that crystallization persists in these glasses despite the lack of visible light scattering. Finally, the combination of both TiO 2 and GeO 2 into a ternary glass also is used to independently tune the dispersion properties of the glass, as demonstrated by measured refractive indices and Abbe numbers, which has potential implications for 3D‐printed optics.

36 MATERIALS SCIENCE↗

Processing and mechanical characterization of short carbon fiber-reinforced epoxy composites for material extrusion additive manufacturing

Fiber-reinforced polymer composites have been extensively utilized in recent years as feedstock materials for material extrusion additive manufacturing (AM) processes to improve strength, stiffness, and functionality of printed parts over unfilled printed polymers. However, the widespread adoption of AM of fiber-reinforced polymer composites requires a deeper understanding of the process-structure-property relationships in printed components, and such relationships are not well understood yet. Fiber length is critically important to the mechanical performance of short fiber composites, but very few studies to-date have focused on how the fiber length distribution (FLD) evolves during processing of composite feedstocks and how this evolution affects printing behavior and mechanical properties in 3D-printed composites. Here, FLD is measured for carbon fiber reinforced epoxy composites over a wide range of ink compositions and shear mixing times, and the distributions are fit with a Weibull-type distribution function. The effects of FLD on the tradeoff between ink processability, ink rheology, printing behavior and mechanical properties are investigated. Furthermore, the effects of printing parameters (nozzle size and print speed) on mechanical anisotropy and fiber orientation distribution (FOD) in printed composites are explored. Mechanical properties of printed composites are characterized via 3 pt-flexural testing, and microstructure is investigated using optical and scanning electron microscopy (SEM), and x-ray computed tomography. Finally, the fitted Weibull parameters are fed into a composite model that incorporates FLD and FOD, and model predictions are found to be in excellent agreement with experimental observations.

3D printing↗