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At least 163 records · Page 9

All-ceramic channel waveguides fabricated via 3D printing

All-ceramic channel waveguides (CWGs) in Yb:YAG transparent ceramics have been fabricated for the first time, to the best of our knowledge, via direct ink write (DIW) and their laser performance has been demonstrated. Single filaments of Yb:YAG nanoparticle-loaded ink were extruded into undoped YAG; the Yb:YAG filaments formed the CWGs, surrounded by undoped cladding. Elemental mapping confirmed the Yb doping profile and waveguide integrity. Optical characterization showed low cladding scatter losses (<1.3%/cm at 1.3 µm), and laser testing with a 940 nm Ti:sapphire pump demonstrated efficient lasing at 1030 nm. The best-performing waveguide, with an elliptical cross-section (100 µm × 60 µm and a length of 1.4 cm), achieved a slope efficiency of 61% and a roundtrip loss of 12.4%. These results identify DIW as a promising approach for fabricating high-performance channel waveguides in transparent ceramics.

36 MATERIALS SCIENCE↗

Fabrication of engineered dopant profiles in Er/Lu:YAG transparent laser ceramics via additive manufacturing

Transparent ceramic Er:YAG laser rods were fabricated via the direct ink write (DIW) method with engineered doping profiles featuring an Er-doped core with endcaps and core-clad structures. Laser rods up to 11 cm in length were produced which required development of a scalable process. To achieve this, multiple improvements were implemented, including printing the rods horizontally on a substrate, rather than vertically, eliminating the need for an external support structure and using a sacrificial drying layer to mitigate warping and defects. Highly transparent rods were achieved with optical scatter levels as low as 0.5%/cm (at 543 nm). A small refractive index difference of 5.7 ppm was measured at the interface between the Er-doped core and the Lu-doped endcaps and cladding. These results demonstrate DIW as a straightforward method for making good optical quality laser rods with engineered doping profiles to improve laser performance.

36 MATERIALS SCIENCE↗

3D printable silicone compositions exhibiting high toughness and low durometer

3D printable silicones can be designed with varying crosslink density, network structures, and types of reinforcing additives. Within this design space, one may tailor the uncured material’s rheology and mechanical response to access a wide range of potential applications. However, printable, low modulus silicones, particularly those applicable to direct ink write, are underreported in published literature. To address the need for higher performance, low modulus silicones with demonstrated printability, a new set of ca. 20–50 Shore A hardness silicone elastomers exhibiting ca. 7 MPa ultimate tensile strength and ca. 400–1200% elongation at break is presented. Mechanical properties were analyzed, providing insight to the effects of formulation constituents on mechanical properties. Cyclic mechanical testing of the silicone formulations was also performed, and the energy loss and permanent set throughout cycling were determined. In conclusion, printed structures demonstrate the feasibility of these new silicones as durable frameworks for novel soft device applications.

36 MATERIALS SCIENCE↗

On the 3D printing of polyelectrolyte complexes: A novel approach to overcome rheology constraints

Strong polyelectrolytes, poly(styrene sulfonate) (PSS), and poly(diallyldimethylammonium) (PDADMAC) dissolved in aqueous KBr can be 3D printed for the first time in the air via direct ink writing (DIW). Viscous polyelectrolyte complex (PEC) solutions were deposited layer-by-layer and quenched with deionized water to produce mechanically viable, viscoelastic hydrogel objects. Optimal inks were confirmed by rheology and thermogravimetric measurements to map flow behavior with material composition. Finally, post-print handling and storage protocols were developed to produce printed resolutions more consistent with conventional DIW.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

VTO FY20Q4 quarterly report

Project Objective.This project has three objectives: (1) tuning microstructures of 3D-printed SSE separators,(2) determining material and processing compatibilities with cathode printing,and (3)3D printing of sintering-free SSE separators.Project Impact.All-solid-state lithium batteries are difficult to process due to the brittleness of ceramic materials, poor solid-solid contact, and electrolyte-electrode stability issues. As a result, the energy and power density and also cycling stability are far from satisfying. This project will address fabrication difficulties by using state-of-the-art 3D-printing techniques that can introduce 3D interfaces and architectures to enhance solid-solid contact and reduce charge transfer resistance. Success will benefit the DOE by establishing the best manufacturing methods for ASSBsto achieve VTO goals on the performance of beyond Li-ion batteries. Approach.The project employs 3D-printing techniques to manufacture SSEs and related components for ASSBs. The team starts with direct ink writing (DIW) to develop ink recipes with desired rheological properties and explore post-sintering approaches to achieve high densification. In parallel with DIW3D printing, the team also explores other 3D printing options, such as projection microstereolithography (PuSL). Both sintering and sintering-free approaches can gain benefit from 3D printing and therefore will be investigated.Out-Year Goals.The team will determine particle sizes and morphologies as well as post-processing conditions that deliver good ionic conductivity and charge transfer properties of LLZTO separators. They will examine co-sintering of LLZTO/cathode and determine the effects of material, particle size, surface coating, and sintering conditions.Collaborations.Microstructures, ionic conductivities, and mechanical properties will be provided to the LLNL simulation team, led by PI B. Wood, for establishing and validating phase-field modeling methods.

36 MATERIALS SCIENCE↗

3D-Printable Inks for Energy and Environmental Applications

Partnering additive manufacturing (3D printing) with functional nanomaterial-based inks has the potential to push the properties and performance of advanced materials beyond previous capabilities. This is particularly true in energy and environmental applications. Graphene, 2D materials, and ceramic-based inks, when coupled with 3D printing technologies like Direct Ink Writing (DIW), also called “robocasting,” have shown promise to greatly enhance the performance of batteries, supercapacitors, reactors, and separator devices. Robocasting enables the printing of large-scale electrodes for energy applications with micron resolution by using high concentration viscous inks.

36 MATERIALS SCIENCE↗

3D printed Ni-Mn-Fe Bi-Functional Catalyst for Metal Air Batteries

Oxygen evolution catalyst with porous structures on the submillimeter and millimeter ranges have been shown to have high catalytic activity. Often, a limiting factor in the performance of a catalyst can be its specific surface area as this can limit the availability of active sites which encourage the desired reaction. As such, the inclusion of a hierarchical structure that include both meso-scale and nano-scale porosity can offer a means to greatly increase the performance of electrochemical catalysts. We have developed a method for manufacturing samples with such a hierarchical structure by combining techniques of direct ink writing (DIW), thermal sintering and free corrosion based dealloying. This allows us to prepare three-dimensionally structured samples with open-cell porosity at the macro-, micro- and nano-scales. Each level of porosity offers a different advantage to the overall functionality and applicability of this technology.

25 ENERGY STORAGE↗

Additively Manufactured, Lightweight, Low-Cost Composite Vessels for Compressed Natural Gas Fuel Storage

This project will develop a process to combine AM via direct ink writing (DIW) technology for CFC printing and to use design optimization tools pioneered at LLNL, with advances in resin/composite formulation enabled by chemical and nano-material modification to produce lightweight low-cost CNG tanks. Our approach will yield sub-scale prototype composite pressure tanks equivalent to Type-5 CNG vessel designs that demonstrate a potential cost-benefit advantage. Central to our vision is using agile AM and design based on computationally informed DIW of both short and continuous CF, further coupled with high-performance thermoset polymer matrixes modified by emergent nanomaterials. Our single-stage, multi-material AM technology, combined with a decreased volume fraction of CF and an increased proportion of economically advantaged short fiber, all together drive the reduction in manufacturing time and overall cost. Importantly, reductions in continuous fiber and overall fiber volume fraction will be achieved without detriment to the mechanical strength of the composite vessel. This will be achieved by employing a single process using multi materials grading involving a thermoset resin “ink” modified with aligned nanoplatelets to leverage the efficient tortuous-path gas barrier effect, printed as an inner flexible gas barrier as the initial stage in our manufacturing process before compositionally grading the AM feedstock in real-time to transition to a rigid, structural CF-filled resin. The proposed hybrid construction is projected to achieve pressure ratings at a service range of 2,900–3,600 psi with a 3× burst safety factor comparable to conventional filament-wound composite tanks with an estimated 30–50% reduction in total manufacturing cost.

03 NATURAL GAS↗

Initial Testing of an In Situ Load Retention Aging Vessel

A thermal aging vessel instrumented with load cells was fabricated. The primary function of the vessel is to continuously monitor the in situ load retention of up to three compressed polymer coupons undergoing thermally accelerated aging under nitrogen. A secondary function is to enable gas sampling of the vessel headspace during thermal aging. Heating of the vessel is achieved using a custom heater jacket. To improve upon our conventional aging study methods which require periodic interruption of aging to perform load testing in an Instron machine at room temperature, this technology aims to automate/facilitate data acquisition/analysis, improve data quality, and enable uninterrupted compression of the polymer which represents the service condition. As an example case to assess functionality of the in situ vessel, the load retention of a siloxane elastomer material additively manufactured by direct-ink-writing (DIW) was measured at three different isothermal aging temperatures for ~1 month. Initial compression of the coupons while near the aging temperature was achieved by temporarily opening the heated vessel to access the interior chamber and manually tightening four nuts to drive the heated compression plate down onto the heated coupons. Initial testing demonstrated achievement of the primary load retention monitoring function. Unfortunately, the vessel leaked which prevented gas sampling; an active purge was used to maintain a nitrogen atmosphere. Welded or otherwise sealed joints, which could be implemented in a future design, would likely eliminate leak paths. To apply time-temperature superposition (TTS), a technique used to provide long-term prediction of the load retention from short-term isothermal data, the load retention needed to be calculated relative to the load at an estimated “equilibrium” time, after most of the transient viscoelastic physical relaxation occurred. The peak load immediately after compression could not be used as the load retention basis for two reasons: (1) age-related changes must be isolated from non-age-related physical relaxation before applying TTS and (2) the manual mechanism used to compress the specimens at the aging temperature was neither smooth nor repeatable which affected the peak load value. To better understand the effect of the mode of initial compression on the measured load, and possibly better estimate “equilibrium” physical relaxation times, systematic stress relaxation experiments were performed using an Instron machine with a thermal chamber. At a given temperature, the DIW polymer was compressed to a fixed strain in either a stepped or continuous manner at two different rates, then held at that strain for 24 hrs. The results indicated that, at a given temperature, the different stress relaxation curves appeared to converge to the same curve at some “equilibrium” time when the non-age-related physical relaxation was mostly complete. Though this observation suggests that the discontinuous manual compression employed by the vessel is feasible, a compression mechanism that is rapid, smooth, and repeatable would enhance its use.

36 MATERIALS SCIENCE↗

Volumetric Additive Manufacturing of Gradient Composition Glass

Advanced optics, such as lasers or cameras, are currently limited by geometric or compositional restrictions on the silica glass components that act as focusing or refracting lenses. Currently, these glass components must be made of one homogenous material in a range of shapes and sizes limited by a few specialized vendors. However, additional flexibility and customization of these optical components could significantly improve the performance of these devices and expand the design space available to optics engineers, as would the capability to locally change the optical properties of these glass components by changing the composition of the glass as a function of location. To this end, we have developed a method to print and process gradient composition glass, using volumetric additive manufacturing (VAM) and direct ink writing (DIW), on-site at Lawrence Livermore National Lab.

36 MATERIALS SCIENCE↗

Virtual Inspection of Advanced Manufacturing via Process-Scale Digital Twins (Abbreviated Report)

Inspection and certification comprise the most significant bottlenecks in advanced manufacturing for NNSA applications, often requiring far more time and resources than the fabrication of the parts themselves. Traditional methods, such as manual review and X-ray computed tomography, are not only slow and costly, but also struggle to provide a clear connection between manufacturing instructions and the final performance of critical components. This gap limits both the agility and assurance needed to support the modernization and safety of the United States nuclear stockpile. In response, our Strategic Initiative established a digital twin framework that integrates realtime process monitoring, automated data analysis, and immersive virtual reality collaboration into a unified inspection pipeline. By leveraging data from sensors, machine instructions, and imaging, we created high-fidelity virtual models of manufactured parts that could be rapidly analyzed and certified. This approach was first demonstrated with Direct Ink Write, and then extended to other manufacturing settings, including conventional (or “subtractive”) manufacturing and to predict the end of life performance of parts per the aging and lifetimes programs. The result is a transformational capability: inspection times have been reduced by a factor of 120,000 without loss of accuracy and while simultaneously improving traceability and confidence in part quality. This framework not only streamlines certification for critical applications, but also positions the national security enterprise to respond more flexibly to emerging challenges, supporting agile manufacturing and digital engineering practices across a broad range of mission-relevant domains.

42 ENGINEERING↗

Development of large-scale, 3D Printed high temperature ceramic material

Through this collaborative effort, a new 3D printing platform for ceramics called laser-induced slip casting (LIS) was explored and developed for improving the processing and manufacture of silicon carbide (SiC), a high temperature ceramic material. This method prints layers of ceramic slips/slurries with subsequent selective-laser heating to dry each layer to build a 3D structure. The completed and dried part is then sintered. This manufacturing process is inherently lower cost than alternative ceramic printing methods such as binder jet technology or stereolithography when it comes to the feedstock material but is more expensive than robocasting or direct ink writing. However, it has the potential to make more controlled parts with less defects compared to robocasting. The largest cost is the heating source for the printer. With this technique, there is potential to make large ceramic parts in a near-net shape. Further, there is no known commercial manufacturing of 3D printed ceramics that creates a large range of different high-density ceramics at large scale. The goals and outcomes for the development of the new printing technology were: 1) assessing the technology with alumina by characterizing coupons, 2) printing and sintering of silicon carbide (SiC), and 3) characterization and properties testing of materials printed and a scale-up of SiC part(s). Through this collaborative project, it was sought to provide the best solution to achieving highly dense and near-net shaped ceramic parts at large scale and reduced cost. The goal was to produce high density sintered materials for applications in defense, energy generating systems, armor, and wear parts using 3D printing methods. Variables including powder particle sizes, dispersant molecular weights (MWs), binders, printing parameters, and post processing were explored as well as the characterization of the physical properties (add specifics here).

36 MATERIALS SCIENCE↗

In Situ Microstructure Characterization of Potassium Di-Phosphate (KDP) Densification during Cold Sintering

In order for ceramic additive manufacturing (AM) to achieve its full potential, it is increasingly important to develop a more rigorous understanding of fundamental phenomena that govern the kinetics and thermodynamics of ceramic AM processes. In the case of additive build processes, such as direct ink write and ceramic extrusion, methods for densifying the resulting green-body product need to be considered to complement the efficiencies of ceramics AM, itself. One densification route, at least for monolithic components, built layer-by-layer, is offered by the recently developed cold sintering process, whereby high-density final product is achieved through addition of a small amount of liquid solvent and application of modest uniaxial compressive stress at relatively low temperature. In situ small-angle X-ray scattering methods and X-ray diffraction have been applied to characterize and quantify the pore morphology evolution during cold sintering for a model system: potassium di-phosphate, KH 2 PO 4 (KDP). It is shown that both temperature and applied stress affect the densification rate, but stress has a stronger effect on the evolving morphology. A regime with an approximate linear densification rate can be identified, yielding an effective densification activation energy of ≈90 kJ/mol.

36 MATERIALS SCIENCE↗

3D Printing of High Viscosity Reinforced Silicone Elastomers

Recent advances in additive manufacturing, specifically direct ink writing (DIW) and ink-jetting, have enabled the production of elastomeric silicone parts with deterministic control over the structure, shape, and mechanical properties. These new technologies offer rapid prototyping advantages and find applications in various fields, including biomedical devices, prosthetics, metamaterials, and soft robotics. Stereolithography (SLA) is a complementary approach with the ability to print with finer features and potentially higher throughput. However, all high-performance silicone elastomers are composites of polysiloxane networks reinforced with particulate filler, and consequently, silicone resins tend to have high viscosities (gel- or paste-like), which complicates or completely inhibits the layer-by-layer recoating process central to most SLA technologies. Herein, the design and build of a digital light projection SLA printer suitable for handling high-viscosity resins is demonstrated. Further, a series of UV-curable silicone resins with thiol-ene crosslinking and reinforced by a combination of fumed silica and MQ resins are also described. The resulting silicone elastomers are shown to have tunable mechanical properties, with 100–350% elongation and ultimate tensile strength from 1 to 2.5 MPa. Three-dimensional printed features of 0.4 mm were achieved, and complexity is demonstrated by octet-truss lattices that display negative stiffness.

36 MATERIALS SCIENCE↗

Inventory Management Improvement Project

The Lawrence Livermore National Laboratory (LLNL) conducts research and development for the National Nuclear Security Agency (NNSA) and its affiliates. The Polymer AM team at LLNL conducts research and development in 3D printing, specifically direct-ink-write, in accordance with LLNL and NNSA missions. The team is composed of machine operators, chemists, testing engineers, and project engineers across multiple lab spaces with one shared storage area at LLNL. The operations use a variety of different consumables and hardware to conduct research applications for LLNL and NNSA. These items are critical to performing operation tasks; if an item is out of stock, operations associated with the respective item could be suspended for weeks. As such, the Polymer AM team manages an inventory of spare consumables and hardware to ensure these items are always available. However, the current management system, an excel sheet managed by the project engineer group, is not intuitive in providing inventory information despite the high labor utilization needed to maintain the system. As such, the team is looking to improve their inventory management that can send notifications regarding inventory needs, accessible to other team members, provide all relevant information to a specific item, and store historical information for budget and operation planning. The proposed solution is a Computer Maintenance Management System (CMMS): a web-based management software that stores inventory information and provides automated notifications. The system will store information on each item including quantity in stock, technical information, supplier information, costs, lead times, and expiration date. The system has a notifications function that can send notifications to the respective team member’s when an item needs to be counted, item inventory is low, or an item is approaching their expiration date. Information for each item can be tracked over time creating data to be used for budget planning and process improvement purposes. Due to its web-based source, the system can be accessed by the respective team member viewing technical information, quantity, and purchasing information.

42 ENGINEERING↗

Additive manufacturing system and method having toolpath analysis

An additive manufacturing (AM) system is disclosed for constructing a three dimensional (3D) part with optimized orthotropy. The system combines an electronic processor which calculates an optimal set of physically achievable toolpaths to meet a given design objective, and a 3D printing direct ink write machine capable of printing inks with reinforcing particles that result in orthotropic materials. The electronic processor may combine a Domain of Interest subsystem that transforms a mathematical description of a desired part orthotropy to a plurality of guidepaths, a toolpath generate subsystem that develops a plurality of physically realizable toolpaths from those guidepaths with a minimum number of starts and stops, a finite element subsystem that computes spatially varying material orthotropy from those toolpaths and then solves a boundary value problem to determine a figure of merit for the design, and an optimization subsystem that uses that figure of merit to update the mathematical description of the part orthotropy to iteratively develop an improved part. The optimization subsystem also includes convergence criteria to indicate when toolpaths have been achieved that yield a sufficiently optimal part has been achieved. The toolpath generate can then output the final toolpaths, which are converted to suitable code that controls the motion of the 3D printer toolhead and allows the optimized 3D part to be manufactured.

King, Michael J.↗

Functional soft materials and methods of making and using thereof

Disclosed are functional materials for use in additive manufacturing (AM). The functional material can comprise an elastomeric composition (e.g., a silicone composite) for use in, for example, direct ink writing. The elastomeric composition can include and elastomeric resin, and a magnetic nanorod filler dispersed within the elastomeric resin. Nanorod characteristics (e.g., length, diameter, aspect ratio) can be selected to create 3D-printed constructs with desired mechanical properties along different axes. Furthermore, since nickel nanorods are ferromagnetic, the spatial distribution and orientation of nanorods within the continuous phase can be controlled with an external magnetic field. This level of control over the nanostructure of the material system offers another degree of freedom in the design of functional parts and components with anisotropic properties. Magnetic fields can be used to remotely sense compression of the constructs, or alternatively, control the stiffness of these materials.

Berkland, Cory↗

Use of latent metathesis polymerization systems for additive manufacturing

The invention is directed to latent metathesis-active resin compositions and additive manufacturing approaches. The latent metathesis-active compositions comprise at least one latent metathesis catalyst, at least one curable metathesis-active monomer, and optional fillers, photosensitizers, and/or a secondary monomer resin system for dual-cure. A method comprises extruding a latent metathesis-active resin from a dispensing apparatus and spatially triggering a ring-opening metathesis polymerization by directed irradiation with light or directed application of a thermal stimuli for direct-ink write printing of objects. Another method uses a latent metathesis-active resin for vat photopolymerization and stereolithographic printing of objects.

Appelhans, Leah↗