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At least 271 records · Page 15

Low-cost sensor-based damage localization for large-area monitoring of FRP composites

Abstract In recent years, there has been growing interest in self-sensing structural materials across research and industry sectors. Detecting and locating structural damage typically requires numerous sensors wired to a data acquisition (DAQ) circuit, rendering implementation impractical in real structures. This paper proposes an innovative, cost-effective sensor network for damage detection and localization in fiber-reinforced polymer composites. The innovation encompasses three key elements: (1) utilizing carbon fiber tows within the composite as piezoresistive sensors, eliminating the need for additional foreign sensor devices; (2) introducing a novel sensor layout wherein sensor tow branches with varied resistance values are connected in parallel, reducing the number of connections to the DAQ circuit and cutting manufacturing costs significantly; (3) developing a practical sensor terminal fabrication technique to minimize manufacturing expenses. The proposed design methodology for the branch resistance values is first validated using a demonstration panel. Subsequently, the overall strategy is assessed by conducting impact tests on carbon and glass fiber-reinforced composite specimens. Results validate the sensor’s ability to accurately detect and locate structural damage.

Demo, Luke B. (ORCID:0000000208806522)↗

Molecular Engineering of Biorefining Lignin Waste for Solid-State Electrolyte

Lignin is the second most abundant renewable biopolymer on Earth but also a waste in both the paper industry and lignocellulosic biorefineries. Recently, lignin valorization has been extensively sought after to return economics, enhance carbon efficiency, and improve the bioeconomy, but the commercial value and size compatibility still hinder its applications. In this study, we developed a facile strategy to apply lignin waste into a solid-state electrolyte (SSE), which represents a safe next generation energy storage. Here, lignin was grafted with polyethylene glycol (PEG), an efficient lithium-ion (Li + ) conductive polymer, to enable its ion conduction. The synthesized PEG-g-lignin was mixed with poly(vinylidene fluoride)-co-hexafluoropropylene (PVDF-HFP) and PEG-g-lignin-based bis(trifluoromethanesulfonyl)imide (LiTFSI) to prepare a solid polymer electrolyte (SPE), which has an ionic conductivity of 2.5 × 10 –5 S/cm at 25 °C. This result was further enhanced to 6.5 × 10 –5 S/cm by adding an ion-conductive ceramic of Li 6.4 La 3 Ga 0.2 Zr 2 O 12 (LLGZO), which is referred to as composite polymer electrolyte (CPE). These data represent the highest ones among reported polymer-based SSE. A mechanistic study by using 2D HSQC NMR revealed that PEG-g-lignin has increased ether type β–O–4 linkages that can promote the interchain hopping of Li+ between lignin polymer chains, and 31 P NMR revealed that the lignin phenolic end can be associated by Li + . Moreover, the abundant aromatic moieties and methoxyl in PEG-g-lignin also enhanced Li + association and improved its ionic conductivity. The superior ionic conductivity of PEG-g-lignin-based SSE can enable massive applications of this biorefining waste in all-solid-state lithium batteries (ASSLBs), which has potential to promote the energy sector by promoting the bioeconomy and enhancing the renewability and sustainability of future energy storage.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Durable polymer-aerogel based superhydrophobic coatings: a composite material

Provided are polymer-aerogel composite coatings, devices and articles including polymer-aerogel composite coatings, and methods for preparing the polymer-aerogel composite. The exemplary article can include a surface, wherein the surface includes at least one region and a polymer-aerogel composite coating disposed over the at least one region, wherein the polymer-aerogel composite coating has a water contact angle of at least about 140° and a contact angle hysteresis of less than about 1°. The polymer-aerogel composite coating can include a polymer and an ultra high water content catalyzed polysilicate aerogel, the polysilicate aerogel including a three dimensional network of silica particles having surface functional groups derivatized with a silylating agent and a plurality of pores.

Kissel, David J.↗

Joining technique for in-oven/autoclave molds manufactured by large scale polymer additive manufacturing

Large scale additive manufacturing (AM) of fiber-reinforced polymer composites has gained traction in the mold and die community over the last decade, largely due to reduced material cost and lead time. However, limitations in mold size remain present due to printer volume constraints and costs associated with large format machines. Here, this paper describes a method for producing additively manufactured polymer molds in segments with an O-ring joint design, which can be machined and subsequently assembled for autoclave applications. The developed joining mechanism allows for maintaining the vacuum integrity during the cure cycle while accounting for the anisotropic nature of the additively manufactured polymer molds. Over a range of tested temperatures, 20–200 °C, the multi-part mold joining design was able to achieve full vacuum of ∼73.7 cmHg (29 inchHg) and maintain a vacuum integrity with vacuum losses less than 1.5 cmHg/5min (0.6 inchHg).

Joining↗

Guidance on the Use of Existing ASTM Polymer Testing Standards for ABS Parts Fabricated Using FFF

When evaluating the static mechanical performance of fused filament fabrication (FFF) polymers, researchers have conducted tensile testing using American Society for Testing Materials International (ASTM) D3039 rectangular test specimens and ASTM D638 Type I and Type IV dogbone test specimens. The choice of ASTM D638 versus ASTM D3039 test specimen geometry is usually based on the perceived susceptibility of the ASTM D638 test specimens to failure within the fillet radius. ASTM polymer and plastic tensile test standards define criteria for acceptably tested specimens as requiring failure inside the narrow length (i.e., ASTM D638) or outside of the grips (i.e., ASTM D3039) for the results to be considered acceptable. There has been limited published research regarding the selection of an ASTM test specimen geometry for FFF polymer materials. This study provides evidence-based guidance through the comparison of the mechanical performance and failure acceptance rates of ASTM D3039 and ASTM D638 test specimen geometries, fabricated using FFF acrylonitrile butadiene styrene (ABS). Here, the purpose of the study is to provide guidance on the use of existing ASTM polymer testing standards for additively manufactured polymers. Results indicate there is an inherent benefit to using ASTM D3039 over ASTM D638 Type I and Type IV test specimens for tensile testing. ASTM D3039 test specimens provide the most consistent failure within the test specimen’s gage length, which is attributed to the rectangular design of the test specimen. Results also indicated that, like traditionally manufactured polymer composites, there will be differences in the tensile test results (e.g., ultimate tensile strength, elastic modulus) based on the different cross-sectional areas of the test specimen geometries.

36 MATERIALS SCIENCE↗

Smart Adhesive Joint with High-Definition Fiber-Optic Sensing for Automotive Applications

Structural health monitoring of fiber-reinforced composite-based joints for automotive applications during their manufacturing and on-demand assessment for its durability in working environments is critically needed. High-definition fiber-optic sensing is an effective method to measure internal strain/stress development using minimally invasive continuous sensors. The sensing fiber diameters are in the same order of magnitude when compared to reinforcement (glass, basalt, or carbon fibers) used in polymer composites. They also offer a unique ability to monitor the evolution of residual stresses after repeated thermal exposure with varying temperatures for automotive components/joints during painting using an electrophoretic painting process. In this paper, a high-definition fiber-optic sensor utilizing Rayleigh scattering is embedded within an adhesive joint between a carbon fiber-reinforced thermoset composite panel and an aluminum panel to measure spatially resolved strain development, residual strain, and thermal expansion properties during the electrophoretic paint process-simulated conditions. The strain measured by the continuous fiber-optic sensor was compared with an alternate technique using thermal digital image correlation. The fiber-optic sensor was able to identify the spatial variation of residual strains for a discontinuous carbon fiber-reinforced composite with varying local fiber orientations and resin content.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Dual C–H functionalization of polyolefins for covalent adaptable network formation via cooperative electrolysis

The increasing demand for carbon fibre-reinforced polymer composites with polyolefin thermoset matrices will lead to the generation of large volumes of low molecular weight waste oligomers during the fibre recovery process. To address this challenge, we present a cooperative electrolytic dual C–H bond functionalization strategy for the one-step installation of two key functional groups essential for dynamic linkages of these deconstructed oligomers. Through direct competition studies, we reveal the predominance of tertiary allylic C–H activation along the complex, branched oligomer backbone. The resulting difunctionalized oligomers form covalently adaptable networks with exceptional circularity. By establishing a sustainable pathway for upcycling deconstructed oligomers from carbon fibre-reinforced polymer fibre recovery, this strategy introduces thermoset materials derived directly from waste. Here, it advances sustainable manufacturing practices, contributing to a net-zero waste synthetic ecosystem, and highlights the prospects of mediated electrolysis in macromolecular transformations.

Electrocatalysis↗

The phantom menace of dynamic soft-shorts in solid-state battery research

Solid-state batteries with lithium metal anodes present the highest energy density batteries for applications in electric vehicles, leading to massive R&D investments over the past decade. Although most research focuses on preventing lithium metal dendrites that eventually short the battery, the nature of these shorts remains elusive. Soft-shorts, in particular, receive little attention or are not recognized, even in published data. Here, in this study, we present a comprehensive outline of the detection and analysis of soft -shorts in solid-state lithium metal cells with composite polymer electrolytes as well as a fundamental understanding of the dynamics of soft -shorts. Transient un-shorting of soft -shorts that occurs on the micro-to-millisecond timescale-driven by joule heating, chemical reactivity, and other processes-limits one's ability to determine whether the cell was or is still shorted. We provide numerous experimental methods to detect and analyze soft-shorts in any battery type as a resource to all battery researchers.

25 ENERGY STORAGE↗

Laponite-Incorporated UiO-66-NH2-Polyethylene Oxide Composite Membranes for Protection against Chemical Warfare Agent Simulants

A strategy is developed to enhance the barrier protection of polyethylene oxide (PEO)-metal–organic framework (MOF) composite films against chemical warfare agent simulants. To achieve enhanced protection, an impermeable high-aspect-ratio filler in the form of Laponite RD (LRD) clay platelets was incorporated into a composite PEO film containing MOF UiO-66-NH 2 . The inclusion of the platelets aids in mitigating permeation of inert hydrocarbons (octane) and toxic chemicals (2-chloroethyl ethyl sulfide, 2-CEES) of dimensions/chemistry similar to prominent vesicant threats while still maintaining high water vapor transport rates (WVTR). By utilizing small-angle neutron scattering, small-angle X-ray scattering, and wide-angle X-ray scattering, the LRD platelet alignment of the films was determined, and the structure of the films was correlated with performance as a barrier material. Performance of the membranes against toxic chemical threats was assessed using permeation testing of octane and 2-CEES, a common simulant for the vesicant mustard gas, and breathability of the membranes was assessed using WVTR measurements. To assess their robustness, chemical exposure (in situ diffuse reflectance infrared Fourier transform spectroscopy) and mechanical (tensile strength) measurements were also performed. It was demonstrated that the barrier performance of the film upon inclusion of the LRD platelets exceeds that of other MOF-polymer composites found in the literature and that this approach establishes a new path for improving permselective materials for chemical protection applications.

36 MATERIALS SCIENCE↗

A Universal Design of Lithium Anode via Dynamic Stability Strategy for Practical All‐Solid‐State Batteries

Abstract All‐solid‐state Li‐metal battery (ASSLB) chemistry with thin solid‐state electrolyte (SSE) membranes features high energy density and intrinsic safety but suffers from severe dendrite formation and poor interface contact during cycling, which hampers the practical application of rechargeable ASSLB. Here, we propose a universal design of thin Li‐metal anode (LMA) via a dynamic stability strategy to address these issues. The ultra‐thin LMA (20 μm) is in situ constructed with uniform highly Li‐ion conductive solid‐electrolyte interphase and composite‐polymer interphase (CPI) via electroplating process. As a result, the passivation layer with poor Li‐ion conduction on Li anode can be dissolved and small surface resistance can be achieved due to the good compatibility of CPI to SSEs. The cycling of Li symmetric cell with Li 6 PS 5 Cl thin film electrolyte (<100 μm) shows a high critical current density of >2.0 mA cm −2 with excellent cycling stability at 1.0 mA cm −2 . The ASSLBs paring with Ni‐rich LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode demonstrated the feasibility of engineered LMA design by presenting good rate capability from 0.1 C to 1.0 C at room temperature, as well as long‐term cycling stability (81 % retention after 100 cycles). This work represents a general pathway to make thin dendrite‐free LMA available for high‐energy‐density ASSLBs.

Deng, Tao [Department of Chemical and Biomolecular↗

A Universal Design of Lithium Anode via Dynamic Stability Strategy for Practical All‐Solid‐State Batteries

Abstract All‐solid‐state Li‐metal battery (ASSLB) chemistry with thin solid‐state electrolyte (SSE) membranes features high energy density and intrinsic safety but suffers from severe dendrite formation and poor interface contact during cycling, which hampers the practical application of rechargeable ASSLB. Here, we propose a universal design of thin Li‐metal anode (LMA) via a dynamic stability strategy to address these issues. The ultra‐thin LMA (20 μm) is in situ constructed with uniform highly Li‐ion conductive solid‐electrolyte interphase and composite‐polymer interphase (CPI) via electroplating process. As a result, the passivation layer with poor Li‐ion conduction on Li anode can be dissolved and small surface resistance can be achieved due to the good compatibility of CPI to SSEs. The cycling of Li symmetric cell with Li 6 PS 5 Cl thin film electrolyte (<100 μm) shows a high critical current density of >2.0 mA cm −2 with excellent cycling stability at 1.0 mA cm −2 . The ASSLBs paring with Ni‐rich LiNi 0.6 Mn 0.2 Co 0.2 O 2 cathode demonstrated the feasibility of engineered LMA design by presenting good rate capability from 0.1 C to 1.0 C at room temperature, as well as long‐term cycling stability (81 % retention after 100 cycles). This work represents a general pathway to make thin dendrite‐free LMA available for high‐energy‐density ASSLBs.

Deng, Tao [Department of Chemical and Biomolecular↗

Biodegradable waterborne polyurethane-urea dispersion adhesives with high biocontent

Non-biodegradable petroleum-based plastic wastes have become a leading environmental concern, and new efforts are underway to prepare biobased and biodegradable replacements. For this work, we have explored the preparation of adhesives suitable for use in consumer products, and here we report the development of waterborne, biodegradable adhesives from biobased monomers resulting in adhesives exceeding 70% biocontent. Using water as the polymer medium, viscosity challenges and the use of volatile organic solvents are avoided. Material properties of the polyurethane dispersions, resulting films, and laminates produced showed M w ranging between 56,000 and 124,000. Lastly, the biodegradability of films and laminates was evaluated. The resulting metrics indicate that the adhesives produced meet the desired mechanical and biodegradability targets, indicating that high renewability content solvent-free polyurethane dispersions are a viable solution for lamination adhesives.

36 MATERIALS SCIENCE↗

Large-scale additive manufacturing tooling for extrusion-compression molds

Carbon fiber reinforced polymer composites (CFPC) have been used in additive manufacturing (AM) due to both the high-strength-to-weight and superior-stiffness-to-weight ratios. CF AM is being considered for tooling applications. In AM, CFPCs are usually aligned along the deposition direction; however, it results in anisotropic thermal properties which affect the heat transfer and warpage of the final part. In this study, three male molds with different infill patterns were produced via the material extrusion additive manufacturing (EDF-AM) process. These include (a) 0°: infill pattern along the printing direction; (b) 90°: infill pattern perpendicular to the printing direction; and (c) 0°/90°: alternate layers along and perpendicular directions. The effect of the infill pattern on thermal conductivity was analyzed and observed that 0° infill (surface temperature: 79.2°C) had the highest conductivity; and 90° infill (surface temperature: 66.4°C) had the least.

36 MATERIALS SCIENCE↗

Linking thermoset ink rheology to the stability of 3D-printed structures

Thermoset polymer composites show promise for additive manufacturing (AM) applications to address some of the limitations of the more widely used thermoplastic feedstock materials. Thermosets offer attractive mechanical properties while providing excellent interlayer bonding, high thermal and chemical stability, and reduced energy consumption as a result of deposition at room temperature. However, since thermoset resins rely on a crosslinking reaction to solidify, rather than quickly cooling like thermoplastics, viscoelastic properties must be relied upon to maintain deposited shape after deposition until crosslinking can occur. This fact has not impeded development and characterization of new thermoset feedstocks on the small scale, but recent efforts to increase scale of thermoset printing have highlighted issues with structural stability under self-weight. This study addresses issues of self-weight by investigating the mechanisms that cause collapse of tall, thin printed walls. Using nanoclay- and fumed silica-filled epoxy feedstocks, this work compares the collapse height for printed walls to stability models based on yielding and buckling mechanics. Inputs for these models – shear yield stress and storage modulus – were taken directly from parallel plate rheometry measurements. Model predictions were found to be in good agreement with experimental results, where both yielding and buckling behavior were observed, provided the rheological properties after a shear excursion were used as inputs. This work establishes a direct link between basic rheological properties of the feedstock, geometry of the printed object, and achievable height. Overall, the results presented highlight the importance of understanding recovery behavior in thermoset feedstocks and provide valuable guidance on the development of more effective direct-ink writing feedstock materials.

36 MATERIALS SCIENCE↗

Vacuum-assisted extrusion to reduce internal porosity in large-format additive manufacturing

Large-scale 3D printing of polymer composite structures has gained popularity and seen extensive use over the last decade. Much of the research related to improving the mechanical properties of 3D-printed parts has focused on exploring new materials and optimizing print parameters to improve geometric control and minimize voids between printed beads. However, porosity at the microstructural level (within the printed bead) has been much less studied although it is almost universally observed at levels of 4 %-10 % when using fiber reinforced materials. This study introduces a vacuum-assist approach that minimizes internal porosity by removing ambient air from the interstitial space between pellets in the hopper and acts as a negative pressure vent for gases that evolve during the initial stages of single-screw extrusion. Vacuum-assisted extrusion was able to reduce porosity below 2 % across a wide range of processing parameters, moisture content, fiber reinforcements, and printing platforms. Specifically, when printing on a large-format extruder (Strangpresse Model-30), the vacuum-assisted extrusion reduced internal porosity by 35–75 % compared to conventional non-vacuum extrusion, and only pores with length scale > 2 microns are affected. The success of this approach prompted the design of a patent-pending continuous vacuum hopper relevant for large-scale 3D printing on commercial systems.

36 MATERIALS SCIENCE↗

Simulation-driven design optimization of reaction injection molding (RIM) process for polydicyclopentadiene (pDCPD): Minimizing cycle time, defects, and warpage

Replacing metal components in trucks, trailers, and buses with lightweight polymer composites is challenging due to high temperatures and complex manufacturing. The Reaction Injection Molding (RIM) process using Dicyclopentadiene (DCPD) resin offers a solution by producing robust parts with excellent stiffness, impact strength, and resistance properties. Simulations are essential for optimizing this process, predicting defects, and improving quality. However, most commercial software is tailored for thermoplastics, requiring thermoset users to generate their own datasets. In this study, a material data card for DCPD was developed to perform RIM simulations. Design of Experiments (DOE) was used to identify key factors affecting filling, curing, and warpage, aiming to minimize cycle time and defects. The simulations explored varying injection gate parameters (size, location, number) and process conditions (mold/resin temperature, injection/curing pressure). Results showed that gate design significantly impacts filling behavior and defects. A single central gate provided balanced flow with fewer defects, while two corner gates led to more defects. Additionally, lower injection pressure increased filling time, while higher mold temperature accelerated curing but led to more warpage. In conclusion, this optimization framework aims to enhance DCPD part performance and promote sustainable manufacturing by reducing waste and energy consumption.

42 ENGINEERING↗

Integrating HPC simulations and physical experiments to characterize the effects of gamma radiation on seismic protective devices

Seismic protective systems, composed of seismic isolators and dampers, can substantially reduce the effects of earthquake shaking on nuclear power plants and components therein. To enable the use of these devices to protect equipment inside a plant and close to a source of radiation, the U.S. Department of Energy (DOE) funded a project at the Idaho National Laboratory (INL) and the University at Buffalo to characterize the effects of absorbed gamma dose on their mechanical properties. An early task in the project was to determine the exposure time required in the INL Foss Therapy Services (FTS) 60 Co gamma irradiator to achieve a target absorbed dose in the materials used to construct isolators and dampers, including fluids, polymers, composites, and metals. This task required the novel integration of high-performance computing (HPC), Monte Carlo N-Particle (MCNP) simulations, and irradiation experiments using Fricke dosimetry. An MCNP model of the FTS irradiator at INL was developed and validated using Fricke dosimetry. Simulations of three experiments in the irradiator, two with Fricke vials only and one with Fricke vials and a large-size isolator, predicted the Fricke-measured absorbed dose rate to within 15% in all three cases, providing high confidence in the calculation of the gamma dose absorbed in the materials comprising the seismic protective devices. The simulations demonstrated that the effects of photon scattering on absorbed dose rate in the FTS irradiator are negligible for test articles installed close to the cobalt sources and near the rear of the irradiator. The validated MCNP model of the FTS irradiator is being used to support ongoing DOE-funded experiments on seismic protective devices and could be applied to future, non-seismic-related experiments. In conclusion, the novel validation process successfully deployed for the FTS irradiator at INL could be applied to other irradiators, requiring new MCNP models and simulations, and irradiation experiments using dosimeters.

42 - ENGINEERING↗

Life cycle cost, energy, and carbon emissions of molds for precast concrete: Exploring the impacts of material choices and additive manufacturing

Molds for precast concrete are commonly used to create simple- to complex-shaped concrete products away from construction sites. These molds are often handmade from wood; however, additively manufacturing (AM, or 3D printing) fiber-reinforced polymer composites is an advantageous alternative, producing significantly more durable, highly complex molds faster, but likely at a higher cost. Here, this study explores the impact of material and production variables on the cost, energy, and carbon emissions of employing composite AM molds over the full lifecycle. The case study employed techno-economic and life cycle assessments to show that using wood flour–poly(lactic acid) or recycled carbon fiber–acrylonitrile butadiene styrene for AM molds can be less expensive than conventional wood molds, especially when considering use phase costs. While wood molds have the least environmental impacts due to wood's higher biogenic carbon sequestration and minimal processing, optimizing AM designs could reduce energy demand, carbon emissions, and cost.

36 MATERIALS SCIENCE↗