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At least 199 records · Page 11

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↗

Printed Electrochemical Sensor for Quantifying Bone Density Loss in Microgravity

Printed electrochemical biosensors have been developed for astronaut point-of-care testing. Our fabrication approach is complimentary with in-space manufacturing for an on-demand and hands-free fabrication process. These sensors are developed using a combination of thin film materials printing and 3D printing and are comprised of carbon nanotube, gold nanoparticle, silver nanoparticle and dielectric inks to make traditional electrochemical sensor devices. Initial prototyped printed electrochemical sensors demonstrate good electrochemical performance while also displaying low batch to batch variability. Here we report the development of a printed sensor to monitor bone turnover. The absence of load bearing forces experienced in microgravity causes a reduction of overall bone mass and results in the development of space osteopenia/osteoporosis.(1,2) Our approach to identify space osteopenia/osteoporosis is to monitor the change in bone mass indirectly through an excreted biomarker of bone remodeling, amino-terminal collagen crosslinks (NTX). Antibodies specific to NTX are added to the sensor’s electrode ink and applied during the manufacturing process. NTX is measured from a urine sample by changes in voltammetry and electrochemical impedance as it binds to the antibody modified electrode surface. The measurement is rapid, quantitative and requires only small handheld electronics to perform the measurement. By this process, ground and flight physicians will receive frequent and real-time insight into the development of space osteopenia/osteoporosis to guide appropriate countermeasures. REFERENCES [1] Nabavi, N. et al (2011) Bone 49, 965-974. [2] Tamma, R. et al (2009) FASEB J 23, 2549-2554.

in-space manufacturing↗

Toward Fully 3D-Printed Two Degree of Freedom Acoustic Liners

An acoustic liner optimization tool is developed for designing two degree of freedom (2DOF) liners with high absorption over a wide range of frequencies and sound pressure levels (SPLs). Two additively manufactured 2DOF liners (one constant and one variable chamber depth) are designed and printed with an embedded perforate layer as the septum. A normal incidence impedance tube study is performed to directly compare impedance and absorption spectra to a more traditionally manufactured 2DOF liner with embedded mesh caps in phenolic honeycomb. Comparisons of test data to predictions are shown as well as SPL sensitivities for each acoustic liner. Broadband absorption is achieved with the 3D printed 2DOF liner containing constant chamber depths, although due to current limitations in printed embedded perforate hole size, not as broad as the traditional mesh cap liner. However, results also show that the 3D printed variable chamber depth sample is more comparable to the mesh cap liner absorption, demonstrating the viability of printed embedded perforates in novel concepts.

acoustic liner 2DOF two degree of freedom 3D print↗

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↗

Two–Photon Printing of Shape–Memory Microstructures and Metasurfaces via Radical–Mediated Thiol–Vinyl Hydrothiolation

Shape-memory resists capable of high-resolution curing into arbitrarily designed structures are increasingly demanded for soft robotics, optical sensors, microscale manufacturing, and biomedicine. Amorphous, shape-memory thiol-vinyl networks were printed using two-photon polymerization (2PP) curing of a simple resin formulated with commercially available reagents. The ability to print high-resolution feature sizes down to 200 nm is attributed to the use of radicalmediated, thiol-vinyl step-growth polymerization that quickly crosslinks the resin, limiting diffusive transport. The thermomechanical behavior of the 2PP-cured material analyzed in compression, tension and three-point bending is similar to the behavior of the UV-polymerized samples. To demonstrate the ability to design, field, and test 4D responsive microstructures, an array of nine springs with coil diameters of 330 μm was printed. Following compressive shapefixing, printed arrays can release 11 μJ of stored elastic strain energy when reheated. Further, a new concept of dichroic-memory of a metamaterial device is demonstrated by printing a twisted woodpile structure with circular dichroism as characterized by Mueller Matrix ellipsometry. Furthermore, our results demonstrate how combining high-resolution 2PP curing with stimuli-responsive molecular architectures can further the engineering of responsive microstructures and metamaterials.

36 MATERIALS SCIENCE↗

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↗

Investigation of interlayer adhesion of 3D printable cementitious material from the aspect of printing process

The safety of structure printed by extrusion-based 3D concrete printing (3DCP) is significantly influenced by interlayer bonding, which is governed by fresh material properties and processes, including mixing, printing, and post-processing phases. Much literature focused on improving interlayer bond strength via material tailoring/bonding agent addition but gave insufficient attention to other phases' impacts. This study investigates the effects of parameters on interlayer bond strength from different phases in 3DCP, including superplasticizer dosage, printing speed, and curing condition. In the mixing phase, the superplasticizer dosage was increased to reduce I{sub thix} and increase surface moisture content (SMC), consequently improving interface microstructure and interlayer bond strength. In the printing phase, similar results were observed by increasing pumping speed to increase material shear rate. In the post-processing phase, proper curing also improved interlayer bond strength. While SMC has a critical impact on interlayer bond strength, material thixotropic index (I{sub thix}) probably has a stronger influence.

36 MATERIALS SCIENCE↗

Quantitative microstructural investigation of 3D-printed and cast cement pastes using micro-computed tomography and image analysis

Highlights: • Processing alters the microstructure in 3D-printed lamellar cubic element. • A unique patterned and connected pore microstructure network exists. • Micro-channels are connected through micro-pores present at interfaces regions. • Three distinct pore volume domains exists in hardened microstructure. • Volume and frequency of pore, hydrated, and unhydrated clusters are dissimilar. Microstructural phases and mechanical properties of lamellar 3D-printed and cast hardened cement paste (hcp) elements were investigated using a lab-based X-ray microscope at two levels of magnification (0.4× and 4×). K-means clustering was used for quantitative image analysis. The entire volume of intact 3-days-old 3D-printed and cast hcp elements was characterized at 0.4× magnification. Three microstructural features (macro-pores, micro-channels, and interfacial micro-pores) were found to reside in three distinct pore size domains. The largest pores of the 3D-printed element were larger than the largest pores of the reference cast hcp element. Moreover, the smallest pore sizes of the 3D-printed element were found to be smaller than those present in the cast counterparts. Micro-channels were found to be connected to one another through the micro-pores present at interfacial regions, indicating the presence of a uniquely patterned and interconnected pore network. The role of locally weak and porous interfaces on mechanical response and fracture properties is discussed.

36 MATERIALS SCIENCE↗

Copper-nickel electroplating of 3D-printed acrylonitrile butadiene styrene for interference and radiation shielding applications

Here, in this study, electromagnetic and radiation shielding structures were fabricated by 3D printing acrylonitrile butadiene styrene (ABS) structures via fused filament fabrication and electroplating with copper (Cu) and nickel (Ni) metals. Prior to electroplating, the printed ABS materials were made conductive by surface electrodeposition of polypyrrole (PPy). ABS adsorbs the pyrrole monomer, which subsequently polymerizes via oxidation forming conductive PPy layer on the printed structures. The successful anchoring of PPy layer can be attributed to its hydrogen bonding and electrostatic interactions with ABS. Thermal analysis, optical, and electron microscopy equipped with energy dispersive X-ray were employed to characterize the printed shielding structures, while the interference and radiation shielding effectiveness were evaluated using a spectrum analyzer and dosimeter, respectively. The interference shielding was found to be effective at 60 ± 5 dB over relatively small frequency range. Shielding was also apparent against gamma and X-ray ionizing rays, but more significantly effective against beta rays. Furthermore, the Cu/Ni coating was able to reduce any heat-induced dimensional changes for the 3D printed ABS substrate without compromising the mechanical integrity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Universal scaling laws of keyhole stability and porosity in 3D printing of metals

Metal three-dimensional (3D) printing includes a vast number of operation and material parameters with complex dependencies, which significantly complicates process optimization, materials development, and real-time monitoring and control. We leverage ultrahigh-speed synchrotron X-ray imaging and high-fidelity multiphysics modeling to identify simple yet universal scaling laws for keyhole stability and porosity in metal 3D printing. The laws apply broadly and remain accurate for different materials, processing conditions, and printing machines. We define a dimensionless number, the Keyhole number, to predict aspect ratio of a keyhole and the morphological transition from stable at low Keyhole number to chaotic at high Keyhole number. Furthermore, we discover inherent correlation between keyhole stability and porosity formation in metal 3D printing. By reducing the dimensions of the formulation of these challenging problems, the compact scaling laws will aid process optimization and defect elimination during metal 3D printing, and potentially lead to a quantitative predictive framework.

42 ENGINEERING↗

Introduction of Chalcogenide Glasses to Additive Manufacturing: Nanoparticle Ink Formulation, Inkjet Printing, and Phase Change Devices Fabrication

Abstract Chalcogenide glasses are one of the most versatile materials that have been widely researched because of their flexible optical, chemical, electronic, and phase change properties. Their application is usually in the form of thin films, which work as active layers in sensors and memory devices. In this work, we investigate the formulation of nanoparticle ink of Ge–Se chalcogenide glasses and its potential applications. The process steps reported in this work describe nanoparticle ink formulation from chalcogenide glasses, its application via inkjet printing and dip-coating methods and sintering to manufacture phase change devices. We report data regarding nanoparticle production by ball milling and ultrasonication along with the essential characteristics of the formed inks, like contact angle and viscosity. The printed chalcogenide glass films were characterized by Raman spectroscopy, X-ray diffraction, energy dispersive spectroscopy and atomic force microscopy. The printed films exhibited similar compositional, structural, electronic and optical properties as the thermally evaporated thin films. The crystallization processes of the printed films are discussed compared to those obtained by vacuum thermal deposition. We demonstrate the formation of printed thin films using nanoparticle inks, low-temperature sintering and proof for the first time, their application in electronic and photonic temperature sensors utilizing their phase change property. This work adds chalcogenide glasses to the list of inkjet printable materials, thus offering an easy way to form arbitrary device structures for optical and electronic applications.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

3D-printed B 4 C collimation for neutron pressure cells

A design for an incident-beam collimator for the Paris–Edinburgh pressure cell is described here. This design can be fabricated from reaction-bonded B 4 C but also through fast turnaround, inexpensive 3D-printing. 3D-printing thereby also offers the opportunity of composite collimators whereby the tip closest to the sample can exhibit even better neutronic characteristics. Here, we characterize four such collimators: one from reaction-bonded B 4 C, one 3D-printed and fully infiltrated with cyanoacrylate, a glue, one with a glue-free tip, and one with a tip made from enriched 10 B 4 C. The collimators are evaluated on the Spallation Neutrons and Pressure Diffractometer of the Spallation Neutron Source and the Wide-Angle Neutron Diffractometer at the High Flux Isotope Reactor, both at Oak Ridge National Laboratory. This work clearly shows that 3D-printed collimators perform well and also that composite collimators improve performance even further. Beyond use in the Paris–Edinburgh cell, these findings also open new avenues for collimator designs as clearly more complex shapes are possible through 3D printing. An example of such is shown here with a collimator made for single-crystal samples measured inside a diamond anvil cell. These developments are expected to be highly advantageous for future experimentation in high pressure and other extreme environments and even for the design and deployment of new neutron scattering instruments.

47 OTHER INSTRUMENTATION↗

Aerosol jet printed 3 omega sensors for thermal conductivity measurement

The 3 omega (3ω) method is a trusted technique for measuring thermal conductivity—a fundamental material property of critical importance in a broad range of applications. However, traditional 3ω sensor processing requires some form of physical vapor deposition, such as metal evaporation or sputtering. These 3ω sensor deposition techniques limit the materials and sample sizes applicable to the 3ω method. This work demonstrates an aerosol jet printing method to directly print silver 3ω sensors that yield accurate temperature-dependent measurement up to 300 °C on materials with thermal conductivity ranging from 1 to 150 W/m K. The interrelationship between printed sensor geometry, sensor thermal stability, and applicability to the 3ω method is examined. Thermal conductivity measurement with 3ω sensors conventionally sintered at 300 °C agrees to independent laser flash measurement within 4% from room temperature to 150 °C. An unconventional rapid high-temperature sintering method is shown to produce sensors that agree within 3% of the laser flash measurements from room temperature to 300 °C. The rapid sintering profiles also reduced the sensor–substrate thermal boundary resistance of the printed sensors by as much as 88%. The direct printing of 3ω sensors creates opportunities for measurement of thermal transport properties in applications previously inapplicable to the 3ω method.

47 OTHER INSTRUMENTATION↗

High-resolution 3D-printed plastic scintillators with tertiary dye

Additive manufacturing offers efficient production of plastic scintillators with nontrivial geometries using vat polymerization, allowing fabrication of geometries which would be difficult or even impossible to produce using conventional subtractive manufacturing. This work presents a novel photocurable scintillator formula that includes coumarin 450 as a tertiary dye to enable high-resolution 3D printing via the manipulation of the 405 nm cure light. Bulk photocured and 3D printed (with and without tertiary dye) samples were compared through observational assessment and spectral response. All samples showed pulse shape discrimination between neutron and gamma events. Inclusion of the tertiary dye has minimal impact on emission spectrum and light output, but significant impact on print resolution as shown by comparison of printed high-complexity geometries and feature resolution test objects. With the use of a cure-limiting dye, unsupported features — such as freestanding pillars — were resolvable down to 0.7 mm. Even finer resolution at or below 0.1 mm was achieved in fully supported, integrated structures printed with off-the-shelf 405 nm desktop 3D printer. Scintillators demonstrated a light output up to 50% of EJ-200 with a PSD figure of merit up to 1.35 at 0.9–1.1 MeVee.

36 MATERIALS SCIENCE↗

Adhesion Testing of Direct-Write Printed Ink on Metallic Structural Components

The successful adoption of additive manufacturing for the rapid prototyping of direct-write printed electronics requires the establishment of quantifiable metrics that can interrogate device performance. One measure of performance is the adhesion strength between the substrate and printed film interface, which is critical since the strength of this interface can dictate the accuracy and reliability of the printed device. In this work, a non-contact laser-induced spallation technique was used to quantify the adhesion of silver printed films on aluminum alloy substrates. The laser-based method was compared to a standardized pull-off adhesion test, which provided baseline measurements of adhesion strength. The sintering conditions were shown to play an important role in the film-substrate adhesion strength, as well as the cohesion and ductility of the film itself. The methods and results described in this work support the establishment of process control steps that are necessary for quickly verifying the reliability of printed devices prior to their deployment in critical experiments.

Adhesion test↗

Qualification of 3-D Printed Mortar With Electrical Conductivity Measurements

Additive manufacturing (AM) or 3D printing of concrete allows for construction of arbitrary shape structures without a mold. Since reproducibility of 3D printed concrete is lower than that of conventional fabrication, each 3D printed structure should be monitored for proper curing. Conventional qualification of concrete is based on several tests, including destructive compressive strength measurements. Because a structure is 3-D printed layer-by-layer, the surfaces of AM concrete structures have significant surface roughness. This limits the applicability of conventional nondestructive testing methods. We investigated qualification of 3D printed mortar by monitoring curing with nondestructive electrical conductivity measurements. Bulk resistance of concrete was extracted from electrochemical impedance spectroscopy (EIS measurements made using custom flexible self-adhesive electrodes, which contour to rough surfaces. We show that bulk resistivity of concrete increases linearly with time. This allows for developing a calibration curve for compressive strength lookup from nondestructive electrical conductivity measurements. Conductivity measurements also allow for estimation of formation factor, which is an indicator of mortar permeability.

36 MATERIALS SCIENCE↗

Mechanical responses of 316L stainless steel printed by wire arc additive manufacturing with different thermal histories

In this paper, 316L stainless steel walls were printed using single-bead pass and multiple-bead pass wire arc additive manufacturing (WAAM), which represent the internal basket wall and external wall of a spent nuclear fuel (SNF) canister; respectively. Scanning electron microscopy (SEM) microstructure characterization and tensile tests at room temperature (21 °C) and elevated temperature (250 °C) were performed on specimens extracted along the length and height directions of the printed walls. Results showed that grain morphology, grain angles, and retained ferrite are different between the two printed walls, which received different heat input in WAAM. The single-bead pass printed wall exhibited higher yield strength than the multiple-bead pass printed wall because of more retained ferrite and larger portion of random-high angle boundaries (RHAB) grains.

Tang, Wei↗

3D Printed Carbon Aerogels for Polymer-Electrolyte Fuel Cells

Carbon aerogels (CA) are known for ultra-low density, very high surface area, fine porous structure, and excellent electrical conductivity. Recent advances in high resolution 3D printing at LLNL enable the manufacturing of complex structured CA electrodes which have been demonstrated in electrolysis, flow battery, and supercapacitor applications. Polymer-electrolyte fuel cells (PEFC) may be an excellent candidate for these materials/methods as designers seek to optimize membrane-electrode assemblies to achieve higher efficiencies. A major challenge to PEFC design is two-phase flow due to water production which causes pore flooding and leads to cell instability and degradation. To mitigate these effects, groups have investigated the creation of liquid specific pathways in the porous layers to alleviate liquid buildup and enhance gas diffusion. While some progress has been made, traditionally manufactured GDLs, which consist of randomly distributed carbon fibers, are limiting. 3D printed CAs are a promising solution as complex macroporous electrode structures can be manufactured out of micro and nano porous filaments with a high level of control. Additionally, the process may allow for the consolidation of multiple layers (MPL, GDL, & flow channels) into a single printed architecture. In this work various CA lattice structures were printed using a direct ink write (DIW) method and liquid breakthrough pressures were measured to demonstrate the ability to tune the water pathways to achieve specific pressure thresholds. Furthermore, a discussion of the prospects for printed CA electrodes in PEFC will focus on material properties, synthesis techniques, and current challenges.

36 MATERIALS SCIENCE↗