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At least 865 records · Page 48

Evaluating Non-Fluoropolymer-Based Co-Extruded Backsheets Using Combined-Accelerated Stress Testing and Materials Forensics

Co-extruded, non-fluoropolymer backsheet films for photovoltaic (PV) modules have gained popularity in recent years based on their cost competitiveness. However, their viability has been thrown into question as a result of widespread, early-life field-failures of some materials, particularly the polyamide (PA)-based “AAA” backsheet product. Failure to detect weaknesses in those earlier products could be due, in part, to insufficient quality testing practices. New testing protocols have recently been developed to better evaluate such materials. Here we show the testing results for a non-fluoropolymer, co-extruded PA-based backsheet film, which demonstrates greater durability than AAA and some commercial fluoropolymers. Using material characterization techniques including Fourier-transform infrared spectroscopy (FTIR), wide-angle x-ray scattering (WAXS), differential scanning calorimetry (DSC), X-ray photoelectron spectroscopy (XPS), elongation-to-break (ETB), and optical microscopy we perform a comprehensive failure analysis to better understand the materials weaknesses. This analysis can ultimately inform how best to improve the material and extend its lifetime. This work serves as a demonstration that some materials should not be discounted due to a single poorly designed product and that more appropriate qualification testing with subsequent materials analysis can be used to develop better materials.

41 EE - Solar Energy Technologies Office (EE-4S)↗

Effect of Alumina Source on the Rate of Melting Demonstrated with Nuclear Waste Glass Batch

The melting behaviors of three glass batches formulated to vitrify high-level waste were compared. These batches, otherwise identical, differed in the alumina source: one was prepared with corundum (Al2O3), another with gibbsite [Al(OH)3], and the other with boehmite [AlO(OH)]. Batch samples, in the form of loose batches or pressed pellets, were heated at 5°C/min up to 1200°C. The expansion of pellets was monitored photographically. Quenched samples of batches, heated in crucibles, were thin-sectioned, investigated with optical microscopy, and analyzed with X-ray diffraction to quantify crystalline phases. Finally, batch-to-glass conversion was investigated with thermal analysis. Corundum was still present in one batch up to 900°C whereas gibbsite and boehmite dissolved below 500°C. In the batch with corundum, quartz, the source of silica, dissolved marginally earlier than in the batches with gibbsite and boehmite. Unlike the batch with corundum that exhibited considerable foaming, the batches with gibbsite and boehmite did not produce primary foam and made a more homogeneous glass. The occurrence of primary foam in the batch with corundum is a likely cause of a low rate of melting within the cold cap of a large-scale electric melter.

Pierce, David A↗

Properties of Geopolymer Composites Reinforced with Basalt Chopped Strand Mat or Woven Fabric

Geopolymers or polysialates are inorganic polymeric, ceramic‐like materials composed of alumina, silica, and alkali metal oxides that can be made without any thermal treatment. Additions of reinforcing phases vastly improve the mechanical properties and high‐temperature stability of the geopolymer. The processing and mechanical properties of both chopped strand mat as well as 2‐D woven fabric‐reinforced potassium geopolymer composites have been evaluated. Hand lay‐up and hydraulic press processing methods were used to produce composite panels. The room‐temperature tensile and flexural strength of chopped strand mat composites was 21.0 ± 3.1 and 31.7 ± 4.4 MP a, respectively, while those of basalt weave‐reinforced geopolymer composites reached 40.0 ± 5.9 and 45.2 ± 9.3 MP a, respectively. Composite microstructures were examined using optical microscopy as well as scanning electron microscopy ( SEM ). Mass, volume, and porosity fractions were also determined. The effect of high‐temperature treatments at 25°C, 300°C, 600°C, and 800°C were analyzed. Finally, Weibull statistical analysis was performed, which showed an increase in reliability when a reinforcement phase was added to K‐geopolymer.

Ribero, Daniel↗

Size effects in 3D–printed polymer–derived, zirconium diboride–reinforced ceramic composites

Preceramic polymers are of interest for use in many manufacturing techniques such as injection molding, ceramic fiber infiltration, and additive manufacturing. However, off-gassing of low molecular weight oligomers occurs when these polymers cure, potentially leading to porosity in the cured part. Here to study how porosity and strength are affected by the size of the printed part, and the presence of a high surface area nano-scale filler, polycarbosilane (PCS) microrods of varying diameter were fabricated via direct ink writing (DIW), an additive manufacturing technique, with two ink formulations containing either zirconium diboride (ZrB 2 ) alone, or ZrB 2 and fumed alumina (FA). Sets of microrods were printed in a range of sizes by using print nozzles of 450, 634, 979, 1 346, or 1 702 μm in diameter, which were thermally cured, pyrolyzed to form ceramic composite microrods, and tested in 3-pt flexure. Porosity increased with increasing diameter, while failure strength decreased. For a given nozzle size, the microrods containing FA displayed lower porosity and higher strength (up to ~500 MPa) compared to the microrods containing only ZrB 2 . Weibull strength analysis was performed on each group of microrods and shows that the addition of FA increased Weibull modulus from 4.63 ± 1.56 to 9.35 ± 0.601. In conjunction with optical microscopy, this analysis indicates two distinct flaw populations in the printed materials, porosity which arises during the curing step and cracking which arises during pyrolysis of the larger specimens.

36 MATERIALS SCIENCE↗

Tailoring Thermal and Mechanical Performance Through Multimaterial Laser Powder Directed Energy Deposition of Copper and 17-4PH Stainless Steel

This study investigates the additive manufacturing (AM) processing, microstructural evolution, and resulting mechanical and thermal properties of multimaterial components combining 17-4PH stainless steel and pure copper (Cu) fabricated via laser powder directed energy deposition (LP-DED). Conventional tooling steels exhibit limited thermal conductivity, significantly constraining production throughput in high-volume processes. Incorporating Cu, with its superior thermal conductivity, could significantly enhance tool performance, though Cu and steel present metallurgical incompatibilities when processed via AM. A systematic investigation was conducted across compositions ranging from 0 to 100 wt% Cu, revealing critical thresholds influencing solidification behavior, defect formation, microstructure, hardness, and thermal transport. Optical microscopy, electron backscatter diffraction (EBSD), hardness testing, and thermal conductivity measurements provided comprehensive process–structure–property correlations. Severe hot cracking occurred at low-Cu contents (6–25 wt%), aligning generally well with crack susceptibility modeling, with an unexpected discrepancy at 25 wt%. Porosity remained low (≥99% dense) throughout the compositional spectrum. EBSD analysis revealed a transformation from columnar martensitic structures at low-Cu contents to equiaxed FCC Cu-dominated structures at higher Cu concentrations, highlighting the complex microstructural transitions driven by Cu-induced changes in solidification and phase stability. Hardness decreased from 330 HV (pure 17-4PH) to 62 HV (pure Cu), consistent with microstructural changes. Concurrently, thermal conductivity improved substantially from 13.5 W/m K to 367.9 W/m K, emphasizing Cu’s dominant role in thermal transport. The findings highlight the feasibility of leveraging compositional gradients between 17-4PH and Cu to achieve tailored tooling with optimized thermal and mechanical performance.

17-4PH↗

Repair strategy for fused silica wedged focus lens with high-density filamentary damage

The National Ignition Facility (NIF) is intentionally operated with the final fused silica glass (SiO2) optics exposed to fluences and intensities with the potential to induce damage that will grow with additional laser exposure. Therefore, the NIF operates a recycle loop to refurbish final optics by mitigating any initiated surface damage to arrest its growth. However, the morphology of filamentary damage, caused by local self-focusing in the bulk of a silica optic, adds complexity to optics mitigation and provides a limitation to optic reusability. Here, we evaluate techniques for mitigating isolated and clustered filamentary damage. Optical microscopy before and after installation on NIF was used to determine the efficacy of filamentary mitigation after a series of high fluence and intensity laser exposures. The challenges and success rate of the methods are compared for various filamentary damage mitigation strategies.

National Ignition Facility↗

Tunable structural color of bottlebrush block copolymers through direct-write 3D printing from solution

Additive manufacturing of functional materials is limited by control of microstructure and assembly at the nanoscale. In this work, we integrate nonequilibrium self-assembly with direct-write three-dimensional (3D) printing to prepare bottlebrush block copolymer (BBCP) photonic crystals (PCs) with tunable structure color. After varying deposition conditions during printing of a single ink solution, peak reflected wavelength for BBCP PCs span a range of 403 to 626 nm (blue to red), corresponding to an estimated change in d-spacing of >70 nm (Bragg- Snell equation). Physical characterization confirms that these vivid optical effects are underpinned by tuning of lamellar domain spacing, which we attribute to modulation of polymer conformation. Using in situ optical microscopy and solvent-vapor annealing, we identify kinetic trapping of metastable microstructures during printing as the mechanism for domain size control. More generally, we present a robust processing scheme with potential for on-the-fly property tuning of a variety of functional materials.

36 MATERIALS SCIENCE↗

Controlling colloidal crystals via morphing energy landscapes and reinforcement learning

We report a feedback control method to remove grain boundaries and produce circular shaped colloidal crystals using morphing energy landscapes and reinforcement learning–based policies. We demonstrate this approach in optical microscopy and computer simulation experiments for colloidal particles in ac electric fields. First, we discover how tunable energy landscape shapes and orientations enhance grain boundary motion and crystal morphology relaxation. Next, reinforcement learning is used to develop an optimized control policy to actuate morphing energy landscapes to produce defect-free crystals orders of magnitude faster than natural relaxation times. Morphing energy landscapes mechanistically enable rapid crystal repair via anisotropic stresses to control defect and shape relaxation without melting. This method is scalable for up to at least N = 10 3 particles with mean process times scaling as N 0.5 . Further scalability is possible by controlling parallel local energy landscapes (e.g., periodic landscapes) to generate large-scale global defect-free hierarchical structures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Bidomain structures formed in lithium niobate and lithium tantalate single crystals by light annealing

The bidomain structures produced by light external heating in z-cut lithium niobate and lithium tantalate single crystals are formed and studied. Interdomain regions about 200 and 40 μm wide in, respectively, LiNbO{sub 3} and LiTaO{sub 3} bidomain crystals are visualized and studied by optical microscopy and piezoresponse force microscopy. Extended chains and lines of domains in the form of thin layers with a width less than 10 μm in volume, which penetrate the interdomain region and spread over distances of up to 1 mm, are found.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Specific features of waveguide recombination in laser structures with asymmetric barrier layers

The spatial distribution of the intensity of the emission caused by recombination appearing at a high injection level (up to 30 kA/cm{sup 2}) in the waveguide layer of a GaAs/AlGaAs laser structure with GaInP and AlGaInAs asymmetric barrier layers is studied by means of near-field scanning optical microscopy. It is found that the waveguide luminescence in such a laser, which is on the whole less intense as compared to that observed in a similar laser without asymmetric barriers, is non-uniformly distributed in the waveguide, so that the distribution maximum is shifted closer to the p-type cladding layer. This can be attributed to the ability of the GaInP barrier adjoining the quantum well on the side of the n-type cladding layer to suppress the hole transport.

36 MATERIALS SCIENCE↗

Wigner Localization and Whispering Gallery Modes of Electrons in Quantum Dots

We used a low temperature near-field scanning optical microscopy (NSOM) to study a formation of Wigner molecules (WMs) in the emission spectra of self-organized InP/GaInP QDs having up to seven electrons. We used a Schottky diode structure for the electrostatic control of the number of the electrons (N) in QD, and we observed the emission of the charged excitons (for N < 3) and of the WMs (for N > 2) in the regime of weak Wigner localization. We show, that a contribution of whispering gallery modes (WGMs) of the electrons and rearrangement of the electrons between the WM and WGM states in the QDs, can explain the anomalous dependence of NSOM image size on the quantum confinement observed for some dots.

36 MATERIALS SCIENCE↗

Anodic Dissolution Rates Accelerate with Decreasing MoS 2 Nanoflake Thickness

Electrochemical gating of 2D transition metal dichalcogenide (TMD) electrodes is an emerging frontier in the field of semiconductor electrochemistry. In this approach, an applied bias modifies the charge carrier concentration of the 2D TMD, causing band edge shifts and drastic changes in charge transfer rates. However, leveraging this effect for (photo)electrocatalysis is practically limited by the stability of the TMD material under gating conditions. Gerischer showed anodic dissolution of bulk TMD electrodes can occur in the dark and hypothesized that the reaction proceeds via an electron tunneling mechanism from surface states to the TMD conduction band [H. Gerischer, D. Ross, and M. Lubke, Z. Physickalische Chem., 139, 1 (1984)]. Here we investigate this possibility in single MoS 2 nanoflakes using in situ optical microscopy and explore whether Gerischer’s electron tunneling mechanism can explain anodic dissolution rates of thin 2D semiconductors. Here, spatially resolved measurements show anodic dissolution initiates at perimeter edge sites and accelerates exponentially with decreasing layer thickness, consistent with Gerischer’s tunneling mechanism. Interestingly, single layer MoS 2 is impervious to anodic dissolution at applied potentials >200 mV more positive than those required to drive dissolution in bulk and multilayer-thick nanoflakes.

2D semiconductor↗

Effect of Electrochemical Charging on Elastoplastic Properties and Fracture Toughness of Li X CoO 2

Mechanical degradation of lithium-ion battery (LIB) electrodes has been correlated with capacity fade and impedance growth over repeated charging and discharging. Knowledge of how the mechanical properties of materials used in LIBs are affected by electrochemical lithiation and delithiation could provide insight into design choices that mitigate mechanical damage and extend device lifetime. Here, we measured Young's modulus E, hardness H, and fracture toughness K Ic via instrumented nanoindentation of the prototypical intercalation cathode, Li X CoO 2 , after varying durations of electrochemical charging. After a single charge cycle, E and H decreased by up to 60%, while K Ic decreased by up to 70%. Microstructural characterization using optical microscopy, Raman spectroscopy, X-ray diffraction, and further nanoindentation showed that this degradation in K Ic was attributable to Li depletion at the material surface and was also correlated with extensive microfracture at grain boundaries. These results indicate that K Ic reduction and irreversible microstructural damage occur during the first cycle of lithium deintercalation from polycrystalline aggregates of Li X CoO 2 , potentially facilitating further crack growth over repeated cycling. Such marked reduction in K Ic over a single charge cycle also yields important implications for the design of electrochemical shock-resistant cathode materials.

36 MATERIALS SCIENCE↗

Inverse Slip Accompanying Twinning and Detwinning during Cyclic Loading of Magnesium Single Crystal

In situ , observation of twinning and detwinning in magnesium single crystals during tension-compression cyclic loading was made using optical microscopy. A quantitative analysis of plastic strain indicates that twinning and detwinning experience two stages, low and high work hardening de-twinning, and pure re-twinning and fresh twinning combined with retwinning. Slip is always activated. For the first time, inverse slip accompanying with pure retwinning and high work hardening detwinning was experimentally identified, which provides insights in better understanding of the activity of twining, detwinning, and slips.

Yu, Qin↗

Vertical z-axis discontinuous carbon fibers for improved lightning strike performance of continuous fiber-reinforced polymer composites

Effective lightning strike protection for critical aerospace and wind applications requires high electrical conductivity to dissipate current efficiently. However, polymer matrix composites face a challenge due to their inherently insulating nature. While conventional carbon fiber-reinforced composites (CFRP) exhibit electrical conductivity in the planar direction, achieving through-thickness conductivity remains an ongoing challenge. In this work, we have undertaken the fabrication of CFRP interleaved with vertically oriented carbon fibers (Z-fiber) to impart higher electrical conductivity along the thickness direction. Two Z-fiber composite variations are prepared: Z-1 with a single layer of Z-fiber and Z-5 with five interleaved layers and compared with no Z-fiber layer (Z-0) composite. The composite panels were subjected to lab-scale lightning strike tests with a current magnitude of 100 kA. To emulate real-world service conditions, an aerospace-grade paint coating was applied to the composite laminates. Comparative analysis shows Z-1 reduces damage diameter to ∼22 mm compared to Z-0 (∼26 mm), while Z-5 exhibits the least damage (∼16.7 mm), confirmed by optical microscopy. Z-5 demonstrates nine times higher through-thickness electrical conductivity than Z-0, reducing electrical anisotropy substantially. Thermal-electric finite element damage modeling predicts surface damage within 6% of experimental values for both Z-0 and Z-5 composites. Flexural tests post-lightning reveal Z-5 retains 66% flexural strength and 86% modulus, significantly better than Z-0, which retains less than 40% for both properties. This study highlights the efficacy of Z-fiber composites in lightning strike protection, offering improved through-thickness conductivity and mechanical property retention.

36 MATERIALS SCIENCE↗

Reactive Extrusion of Waste Plastics with Compatibilizer and Lightly Pyrolyzed Crumb Rubber for Asphalt Modification

Modifying asphalt is a potentially high-value application for reusing waste plastics because of the high-volume usage of asphalt in highway construction. However, simply blending hot plastics and asphalt encounters difficulties related to the poor solubility of polymers, which limits the formation of a swollen network with asphalt molecules. The polymer phases also tend to coalesce and separate from asphalt during high-temperature storage in static conditions. The present study developed an innovative process to stabilize waste plastics in asphalt and improve binder storage stability by using lightly pyrolyzed crumb rubber together with a chemical compatibilizer. Both polymers were extruded to produce a thermoplastic elastomer (TPE) for asphalt modification. The mechanical performance and chemical reactions of TPEs were characterized via tension test and Fourier transform infrared spectroscopy. The storage stability and rheological properties of modified binder blends were evaluated through laboratory asphalt stability test and dynamic shear rheometer test. Polymer phases and network structures were characterized through optical microscopy. It was found that the pyrolyzed and reactive extrusion process improved the rubber solubility and polymer interaction, and therefore the storage stability of modified binder blends. The co-existence of rigid plastic and soft rubbery regimes in an entangled network provided a promising pathway to improve the mechanical performance of asphalt binders in both high- and low-temperature domains.

Ma, Yuetan↗

Characterization and repair of core gap manufacturing defects for wind turbine blades

Various wind turbine blade components, such as shear webs and skins, commonly use fiber-reinforced composite sandwich structures with a core material like balsa or foam. During manufacturing, core gap defects may result from the misalignment of adjacent foam or balsa core sheets in the blade mold. It is important to understand the influence that core gaps have on the structural integrity of wind turbine blades and how to mitigate their influence. This research characterized the effects of core gap defects at the manufacturing and mechanical levels for both epoxy and next-generation thermoplastic composites. Common repair methods were assessed and compared. Multiple defect sizes were compared using temperature data gathered with thermocouples embedded during manufacturing to core gap defect characteristics obtained using image-mapping techniques, optical microscopy, and mechanical characterization by long beam flexure. Results showed that peak exothermic temperatures during curing were closely related to core gap size. The long beam flexure tests determined that transverse core gaps under pure bending loads can have a substantial effect on the ultimate facesheet strength of both epoxy and thermoplastic composite sandwich structures (up to 25% strength reduction), although the size of the defect itself had less of an influence on the magnitude of the strength reduction. The supporting image-mapping techniques indicated that the distortion of the composite facesheets by the core gaps contributed to the premature failures. The repair methods used in this study did very little to improve the ultimate strength of the sandwich panels that previously had core gap defects. The repair of the thermoplastic panel resulted in a further loss in ultimate facesheet strength. This research demonstrated that there is a vital need for the development of a compatible thermoplastic polymer repair resin system and appropriate resin specific repair procedures for the next generation of recyclable thermoplastic wind blades.

17 WIND ENERGY↗

Accurate measurement of porosity size and morphology in aluminium alloy laser welds

Conventional two-dimensional optical microscopy is the most common tool for capturing and quantifying keyhole collapse porosity and other defects formed during the laser welding of aluminium alloys. This approach is of limited utility since only a single longitudinal or transverse metallographic cross-section, comprising only a small fraction of the overall weld volume, can be extracted or analysed at a time. X-ray computed tomography tools, on the other hand, enable three-dimensional visualisation and analysis of porosity and defects to be made across the full weld volume. When comparing these two measurement techniques, two-dimensional microscopy tools significantly underestimated the fraction of defects present within the weld at levels between 50% and 80%. Three-dimensional x-ray computed tomography tools also provide a means for accurately characterising the location, size and morphology of irregularly shaped defects. By categorising the defect shapes using a Zingg's shape analysis, in which the distribution of defect morphologies could be quantified as disk, rod and spherical shapes, a transition in defect morphology moving from stationary beam to oscillating beam welds was detected and quantified.

36 MATERIALS SCIENCE↗