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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Delamination recycling of multilayer plastic films: Solvent-assisted separation pathways and recovery of solid polyolefins

Multilayer plastic films are excellent packaging materials due to the bound layers of multiple polymers, with each different polymer contributing to the film properties. Desirable properties lead to continuously growing demand for multilayer films. Multilayer plastic films are typically single-use and, as such, their increased production and disposal have led to waste management problems. Multilayer films are not currently recyclable primarily due to the multiple bound polymers. This work advances delamination as a recycling process to separate and sequester valuable polymers from multilayer films, facilitating the incorporation of these polymers into the circular economy. We effect delamination in a physical process that preserves targeted polymers as solid film, hence retaining their embodied energy. This work documents three different pathways of inducing delamination of multilayer films, with appropriate solvents disrupting adhesion between adjacent layers or dissolving a minor component of the film in less than an hour and at temperatures below 90°C, and where all initial polyethylene is maintained in its solid form throughout the process and is recovered at high purity. Solvent-based delamination is exemplified on commercial multilayer films with majority polyethylene (PE), and polyethylene terephthalate (PET) or ethylene vinyl alcohol copolymer (EVOH) or nylon also present. Solvent-based delamination is an energy-efficient and environmentally friendly recycling process that improves upon dissolution-precipitation recycling, since delamination involves very little dissolution and no precipitation, and is superior to pyrolysis which breaks down the polymers, while delamination keeps polymer chains intact. Furthermore, delamination recycling can contribute to the sustainable use of multilayer films as they continue to protect our food and medicine.

Chemical Recycling↗
DOE OSTI2025

Delamination-informed lifecycle decisions: A dielectric and machine learning framework for composite sorting and recycling

Composite materials are widely used in aerospace, marine, and automotive sectors due to their high strength-to-weight ratio and durability. However, their long-term reliability can be compromised by damage accumulation. Specifically, delamination initiation serves as a precursor to structural failure, which is often difficult to detect during damage inspection. Identifying and sorting delamination initiation in samples not only increases operational safety while providing critical information for end-of-life decisions, which influences both the service life extension value and the efficiency of fiber extraction during recycling. This research addresses two challenges: (1) developing a nondestructive, ex-situ framework to sort composite materials based on damage severity, particularly delamination, and (2) understanding how damage in composites influences resin removal during pyrolysis. Both experimental work and finite element analysis were performed to predict critical stress levels that are associated with delamination onset. Based on these results, three loading levels 50 %, 75 %, and 90 % of maximum stress, were selected for controlled experiments, generating composite samples with varying extents of damage for machine learning model training. Microscopic imaging of these samples confirmed the damage progression from matrix cracking to delamination, validating the computational predictions. We explored supervised machine learning using dielectric measurements to classify damage states. Preliminary results show an artificial neural network can identify early delamination which is a potential precursor to failure, with 94.44 % accuracy on our dataset. A parallel investigation into the effect of damage severity on pyrolysis recycling showed that heavily delaminated samples required significantly less energy for comparable matrix removal than undamaged samples.

dielectric variables↗
DOE OSTI2025

Minimization of Cathode|Solid-Electrolyte Interfacial Delamination through the Application of Interphase Layers

Next-generation lithium-ion batteries are expected to use solid electrolytes (SEs) to enable higher energy density and extreme fast-charge capabilities. One major mode of degradation at the cathode|SE interface is delamination between the cathode active materials and SEs, which leads to performance decay. Experimental observations indicate that implementation of interphase layers can minimize the cathode|SE delamination induced capacity fade. A multiscale computational methodology is developed here to investigate the applicability of boron substituted lithium carbonate (Li 2+x B x C 1–x O 3 , x = 0.5, or LBCO) to minimize the delamination at the cathode|SE interface. Atomistic simulations indicate that the fracture energies at both the cathode|LBCO and LBCO|SE interfaces are higher than those at the cathode|SE interface, which reduces the extent of delamination. Mesoscale simulations indicate that, apart from increasing the fracture energy, decreasing the evolution of strain energy by lowering the elastic modulus of the interphase layer can also minimize the extent of delamination at the cathode|SE interface. However, the adoption of an interphase layer with high ionic conductivity is necessary to minimize the ohmic losses during operation at higher current densities. This study provides guidance on selecting interphase layers with specific properties and thicknesses to minimize both interfacial delamination and impedance growth.

LBCO↗
DOE OSTI2026

Delamination of Multilayer Plastic Films to Recover Polyethylene with Favorable Mechanical Properties

Multilayer plastic films play a critical role in packaging, with each polymer layer contributing specific properties to the multilayer film. Multilayer plastic films are not currently recyclable due to the bound polymers. With multilayer film production of about 20 million metric tons in 2024 and rising, endof- life treatment becomes pressing. This work presents a scalable solvent-based delamination recycling process that is applied to commercial postindustrial multimaterial films to unbind the materials within a multilayer film by dissolving only the adhesive layer and recover polyethylene (PE) as an intact solid film. Solventbased delamination is a simple process that allows the complete recovery of materials and solvents used in the process. The delaminating solvent, 88% formic acid in water, induces delamination of PE/PEI/PET and PE/PU/PET films at 70 °C in under an hour. Recovered PE has no contamination detected by Fourier transform infrared spectroscopy and mechanical properties on par with those of virgin resin. The recovery of high-quality solid PE film fit for reprocessing, at low operating temperatures and with closed-loop solvent reuse, promotes delamination as a low energy consumption and environmentally friendly recycling process. PE recovered from delamination can be reused in equivalent products, promoting circularity of multimaterial films.

chemical recycling↗
DOE OSTI2026

Effects of stabilizer strength on the delamination strength of ReBCO coated conductors

Delamination strengths (DSs) of ReBCO tapes were evaluated using a transverse tensile anvil test. This study first demonstrated that the electromechanical DS is nearly equivalent to the purely mechanical DS for ReBCO tapes exhibiting abrupt delamination behavior. Mechanical DS was then examined for tapes with and without stabilizer edges to assess the influence of stabilizer strength. Scanning electron microscopy/energy-dispersive x-ray spectroscopy analysis revealed the delamination sites and crack propagation in ReBCO tapes. Further investigation revealed that the DS of ReBCO tapes is primarily determined by two factors: (1) interfacial bonding strength between the layers and (2) mechanical strength of the stabilizer edges. These findings point to a potential approach to enhancing DS by increasing the strength of the stabilizer (e.g. by optimizing the Cu electroplating process).

Cu stabilizer↗
DOE OSTI2025

Microstructure-based modeling of inner oxygen pressure in solid oxide electrolysis cells: Analysis of electrode delamination and mitigation

One major degradation mechanism during long-term operation of solid oxide electrolysis cells (SOECs) is delamination of oxygen electrodes (OEs). The driving force for the electrode delamination could be the generated high inner oxygen pressure near the electrode-electrolyte interface during operation. However, the effects of transport properties and electrode thickness on the inner oxygen partial pressure are not well understood. Here a microstructure-based electrochemical model, which includes the conduction of electrons and oxygen ions coupled with Butler-Volmer-type chemical reactions at triple-phase-boundaries (TPBs), is employed to investigate the oxygen pressure in lanthanum strontium manganate (LSM)-based SOECs. The model is applied to both two-dimensional (2D) prototype microstructures and three-dimensional (3D) realistic microstructures, and the oxygen pressure is analyzed as a function of transport properties and electrode thickness under both potentiostatic and galvanostatic operations. The simulation results suggest strategies to suppress electrode delamination. The simulation results are compared to an analytical solution, and the discrepancies are attributed to the Butler-Volmer-type kinetics included in the microstructure-based model.

25 ENERGY STORAGE↗
NASA NTRS2020

Evaluation of Fatigue Damage Accumulation Functions for Delamination Initiation and Propagation

The present report follows on the cohesive fatigue damage model methodology proposed in NASA-TP-2018-219838. In that report, an empirical function describing the incremental damage due to cyclic loading was used to calculate fatigue damage within a cohesive formulation. The form of the function was developed such that, when integrated at a constant stress amplitude from no damage to failure, it produces a life versus load response that is consistent with an S-N diagram. Therefore, the parameters of the damage model could be obtained by fitting the model predictions to an S-N diagram. The finite element analyses performed demonstrate that the cohesive fatigue accumulation function provides a link between the S-N diagram that describes crack initiation, and the Paris law that characterizes the rate of crack propagation. However, when the model was proposed, it was not known whether the form of the damage accumulation function associated with a desired S-N diagram is unique and, if not, if the link between S-N and the Paris law is unique and independent of the fatigue function selected. In the effort described herein, several alternative forms of the damage function that reproduce the desired features of S-N diagrams were found and evaluated. The effects of each of these functions on the predicted parameters of the Paris law and the propagation threshold are discussed. The results indicate that the predicted exponent m of the Paris law is indeed independent of the damage accumulation function. However, different functions predict different values for the pre-factor C of the Paris law. Therefore, the proper damage accumulation function must be selected by comparison with experiments. One of the new damage accumulation functions proposed herein was found to be particularly useful for analysis because of the ease with which the model parameters can be determined with a minimal amount of experimental information. The effectiveness of the proposed methodology and damage function was demonstrated by conducting analyses of a double cantilever beam test, a mixed-mode bending test, and a three-point bending test of a skin/doubler specimen. The results indicate that the same set of model parameters can provide accurate predictions of the rate of fatigue crack propagation for a variety of material interfaces, mode mixities, load levels, and stress ratios.

DKIN/Stiffener Debonding↗
DOE OSTI2026

Fracture Analysis of Cohesive Zone Models for Modeling Residual Stress Induced Delamination in Composite Structures

A fracture study of coupon-scale composite cylinders with embedded defects was conducted with an objective to assess and validate a modeling approach using two available cohesive material models. The study included experimental and simulation evaluations of initiation of crack growth and progression. Interrupted thermal experiments used acoustic emissions monitoring to identify the onset of crack progression during each cooling interval and ultrasonic scanning provided images of defect growth. Verification, validation, and uncertainty quantification (VVUQ) processes were performed in the assessment of the simulation predicted temperature at which crack propagation begins (quantity of interest). The Sobol sensitivity analysis identified the hoop direction elastic modulus in the carbon fiber reinforced polymer (CFRP) plies as the most influential parameter for simulations using both cohesive models, accounting for at least 70% of the variation in the temperature at crack propagation. The UQ temperature range for the Tvergaard-Hutchinson model was higher (more conservative) than the experimental acoustic measurement indicators of crack progression, while the temperature range for the Thouless-Parmigiani model enveloped the experimental data points for the primary defect size of 0.75 x 1 in. The simulations could not capture the stable crack growth indicated in the experiments. This is likely due to the models’ inability to represent anisotropic fracture toughness attributed to the structure of the orthotropic fiber weave in a woven composite laminate.

42 ENGINEERING↗
DOE OSTI2025

Simultaneously improved reversibility and hydrogen production of solid oxide cells through infiltrating air electrode

Among the various fuel cells, solid oxide cells (SOCs) are the unique type that can principally operate reversibly as either fuel cells to produce electricity or as an electrolyser to split water and produce green hydrogen (H 2 ). Nevertheless, the SOCs' reversibility presents enormous challenges that are manifested by the fast degradation through the cycling between fuel cell and electrolysis mode. While the La 0.8 Sr 0.2 MnO 3 /yttria-stabilized zirconia (LSM/YSZ) air electrode possesses significant advantages in terms of high electrical conductivity and high thermal stability under fuel cell mode, the SOCs with the LSM/YSZ air electrode experience rapid performance degradation with catastrophic electrode delamination shortly after switching from fuel cell to electrolysis mode. To prevent such catastrophic delamination and enable the electrolysis H 2 production, a chemical solution with the designed chemistry of SrFe 2 O 4-d was infiltrated into the LSM/YSZ air electrode. The infiltration immediately mitigates the catastrophic delamination, and the infiltrated cells exhibit significantly improved reversibility upon the electrochemical operation. Nanostructure examination reveals nanoscale cracks and second-phase nanograins formed in the air electrode from the baseline cell. By contrast, no delamination was observed at either the micron or the nanoscale for the infiltrated cell, which is attributed to the increased ion conductivity of the Fe-doped LSM mixed conductor induced by the significant interdiffusion between the LSM backbone and infiltrates. Here, this study presents a viable method for preventing electrode delamination while enhancing the durability of H 2 production and power generation for reversible fuel cell/electrolysis cell operation. It further opens new research directions of modifying the electrochemical activity of the electrode of inherently functional cells through the infiltration of the solutions with different chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Recovery of terephthalic acid from solar PV backsheets using waste solvent from distilled spirits production

Current research on solar photovoltaic (PV) recycling mainly focuses on recovering valuable metals and glass, often neglecting the polymeric components, particularly the backsheets, which are typically landfilled or thermally decomposed. This study explores an innovative approach to upcycle PV backsheets into value-added products, specifically terephthalic acid (TPA), using waste ethanol solvent from the distilled spirits industry. Experimental results show that increasing both exposure time and ethanol concentration significantly enhances backsheet delamination efficiency. Using waste ethanol, a maximum delamination efficiency of 80% was achieved at room temperature after 24 hours. In decomposition trials, both sodium hydroxide (NaOH) and potassium hydroxide (KOH) demonstrated comparable efficiencies (96.6–97.5%) over 8 and 24 hour reactions. With virgin ethanol, NaOH yielded 94–97.5% TPA recovery. Notably, using waste ethanol achieved a TPA recovery efficiency of 96.8%, underscoring the process's economic viability and sustainability. Analytical characterization of TPA recovered after 8 hours showed consistent spectral patterns across both alkalis and solvents, indicating a similar chemical environment and functional groups. The recovered TPA can be repolymerized into high-purity PET, suitable for manufacturing new PV backsheets. This work advances polymer-recycling by demonstrating that an industrial waste solvent (distilled-spirits ‘heads’) can replace virgin ethanol without loss in delamination performance or TPA yield. While PV backsheet PET is a modest share of global PET, using waste ethanol to upcycle this currently under-recycled stream demonstrates a transferable solvent-reuse pathway that can extend to higher-volume PET sources.

Nain, Preeti [Michigan State Univ., East Lansing, ↗
DOE OSTI2025

Hierarchical domain structures in buckled ferroelectric free sheets

Flat elastic sheets tend to display wrinkles and folds. From pieces of clothing down to two-dimensional crystals, these corrugations appear in response to strain generated by sheet compression or stretching, thermal or mechanical mismatch with other elastic layers, or surface tension. Extensively studied in metals, polymers and, — more recently — in van der Waals exfoliated layers, with the advent of thin single crystal freestanding films of complex oxides, researchers are now paying attention to novel microstructural effects induced by bending ferroelectric-ferroelastics, where polarization is strongly coupled to lattice deformation. Here we show that wrinkle undulations in BaTiO3 sheets bonded to a viscoelastic substrate transform into a buckle delamination geometry when transferred onto a rigid substrate. Using spatially resolved techniques at different scales (Raman, scanning probe and electron microscopy), we show how these delaminations in the free BaTiO3 sheets display a self-organization of ferroelastic domains along the buckle profile that strongly differs from the more studied sinusoidal wrinkle geometry. Moreover, we disclose the hierarchical distribution of a secondary set of domains induced by the misalignment of these folding structures from the preferred in-plane crystallographic orientations. Our results disclose the relevance of the morphology and orientation of buckling instabilities in ferroelectric free sheets, for the stabilization of different domain structures, pointing to new routes for domain engineering of ferroelectrics in flexible oxide sheets.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Impact of droplet oxidation on mechanical properties of an Al-7Si-0.4Mg alloy fabricated with liquid metal jetting

Droplet-on-demand liquid metal jetting (DOD-LMJ) is a new method for additive manufacturing of bulk structural alloys. Here, we report on the microstructure, tensile, and fatigue properties of an Al-7Si-0.4Mg (A356) alloy fabricated with LMJ. Liquid metal droplets were shielded by high-purity Ar gas shroud during deposition. Atom probe tomography revealed that a few nanometers thick (Al-Mg-Si)-O oxide film formed on the droplets despite Ar gas shielding. Tensile tests on peak-aged LMJ A356 alloy showed that yield strength was isotropic (250 MPa), but ductility was lower in the build direction (6.1 ± 1.4 %) compared to the transverse direction (9.4 ± 1.0 %). Lower ductility in the build direction was attributed to delamination of metal-oxide interfaces at layer boundaries. The ductility and yield strength of LMJ A356 were similar to cast A356 and laser powder bed fused (LPBF) A357 alloys, indicating the limited impact of oxide film on tensile properties. The oxide film severely impacted the fatigue properties. Fatigue resistance of LMJ A356 was limited by fatigue crack initiation at lack-of-fusion defects and fatigue crack propagation along layer boundaries by delamination of the metal-oxide interface. The fatigue strength of LMJ A356 at 60 MPa was lower than cast A356 and LPBF A357 alloys in the peak-aged condition. This research underscores the need for managing droplet oxidation during LMJ additive manufacturing of structural alloys.

42 ENGINEERING↗
DOE OSTI2026

Characterization of Electronic Stress-Induced Changes in Multilayer MoS 2

Transition metal dichalcogenides like molybdenum disulfide (MoS 2 ) are compelling for next-generation electronic devices. In this work, we investigate the impact of electronic stress on MoS 2 to illustrate that observational and phenomenological information on multiple devices can be useful to describe changes in the device, and caution against the rationalization of paltry results as representative or correlative to device behavior. Here, we stress MoS 2 by applying a sustained 20 V DC bias to study the material’s response. Post-stress electronic characterization revealed nonuniform shifts in current–voltage (I–V) behavior alongside microscale changes. Complementary mechanical, spectroscopic, and scanning microwave impedance measurements showed that stress-induced features locally modulate stiffness, surface potential, Raman intensity, and charge carrier density. We correlated I–V behavior with morphological features (wrinkles, tears, folds, height) and device-level geometry (MoS 2 overlap with electrodes, channel area, contact length) on 50 test structures across five chips to move beyond anecdotal conclusions. We found no universal correlations before DC stress. However, device-level geometry was correlated with I–V behavior after DC stress, suggesting that electrode contacts play a more dominant role than morphology in determining performance. Delamination and thinning induced by DC stress led to localized reductions in charge carrier density within the affected regions. Further, delamination and thinning appear to map to I–V device performance in a few samples, but the correlation is lost when a larger sample size is considered. This suggests significant sample-to-sample variability in surface electronic states of the test structures. We also discuss how environmental factors introduced during fabrication may contribute to the observed heterogeneous device response. Progress will require high-resolution, multimodal analysis across many samples constructed under controlled, clean conditions. By building data sets that capture variability, we can better identify the true drivers of performance.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Chemo-Mechanical Behavior and Stability of High-Loading Cathodes in Solid-State Batteries

Solid-state batteries can offer higher energy density and improved safety compared to lithium ion batteries, which use flammable liquid electrolytes. Increasing the ratio of cathode active materials in composite cathodes enhances the energy density and reduces manufacturing costs. Changes in the ratio of cathode active materials alter the microstructure and chemo-mechanical response of a cathode during operation. Understanding the relationship between composition, microstructure, and chemo-mechanical interactions is critical for optimizing solid-state cathodes. Here, in this study, we engineered composite cathodes with varying ratios of LiNi 0.8 Co 0.1 Mn 0.1 O 2 and Li 6 PS 5 Cl to systematically investigate the role of microstructural evolution in long-term chemo-mechanical transformations. Chemo-mechanical stresses resulting from the volume changes of the cathode active materials led to degradation mechanisms, such as fracture and interfacial delamination. Active material fracture and delamination led to underutilization of active material and significant capacity decay during cycling. Coatings that suppress active material-active material interactions during cycling may aid in suppressing the generation of local stress hotspots.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Infrared thermography NDT for in-situ defect detection in sandwich composite panel manufacturing

Composite manufacturing presents numerous challenges, as defects can arise from various sources throughout the process. In sandwich composite structures, the integration of a foam core introduces additional complexity and increases the likelihood of defect formation like delamination. To mitigate these issues and reduce the risk of future structural failures, in-situ monitoring during manufacturing is essential. This study investigates infrared (IR) thermography as a non-destructive technique for detecting manufacturing defects in foam-core sandwich composite panels under thermally excited conditions representative of in-situ processing. A stationary FLIR A8590 IR camera (640 × 512 pixels, 30Hz, 17mm lens, 9 ft stand-off distance) was used to monitor prefabricated panels subjected to controlled external heating simulating compression molding and resin cure exotherm. Interlaminar delamination defects with characteristic sizes ranging from 0.25 × 0.25in² to 5 × 5in² produced measurable surface temperature depressions of approximately 4–10°C during transient cooling, exceeding the effective noise floor of the camera by more than two standard deviations. Thicker laminates exhibited prolonged defect detectability windows due to increased thermal diffusion time. In contrast, embedded Teflon inclusions generated weak thermal contrasts of ≤ 3°C, approaching the measurement noise floor, due to limited thermal property contrast with the surrounding glass fiber composite. These results establish quantitative detectability limits for stationary thermographic inspection of sandwich composite panels under manufacturing-representative thermal cycles.

Barakat, Abdallah [ORNL] (ORCID:0000000296141398)↗
NASA NTRS2026

Fatigue Life of Flow-Formed Aluminum 2195 and 6061 Alloys

The successful design and fabrication of metallic cryotanks for commercial aviation applications require lightweight, durable materials capable of withstanding high pressures and cryogenic temperatures through tens of thousands of thermomechanical refueling cycles. Flow forming is an advanced manufacturing technique that offers high-rate production and scalability for fabricating integrally stiffened cylinders suitable for cryotank applications. This work establishes the durability of flow-formed aluminum alloys by characterizing their fatigue life performance under conditions that mimic cryotank refueling cycles. Residual stresses in flow-formed aluminum-lithium (Al-Li) 2195-T6 cylinders were assessed using the contour method and found to be minimal. Fatigue life testing was conducted on flow-formed Al-Li 2195-T6 at room temperature and cryogenic temperatures (-321°F [-196°C]), with wrought Al-Li 2195-T6 serving as a baseline for comparison. Results showed that flow-formed materials exhibited fatigue performance comparable to or better than wrought materials, with no statistically significant differences observed between different specimen orientations relative to processing directions. Fractography revealed reduced delaminations in the flow-formed Al-Li 2195 samples as compared to wrought, indicating potential improvement to the microstructure that could result in improved service properties. Texture analysis using electron backscattered diffraction (EBSD) indicated recrystallization during heat treatment, potentially contributing to reduced delamination susceptibility. These findings demonstrating flow-formed material durability coupled with the high manufacturing efficiency of flow forming, makes flow forming an attractive process to produce aircraft cryotanks.

EBF3↗
DOE OSTI2025

Influence of build direction on the fracture mechanism of 3D printed octet lattices

Here, we investigate the effects of 3D printing build directions on the fracture properties of octet lattice metamaterials made of polylactic acid (PLA) and how these effects vary with the relative density of the lattices. Single-edge notch bend samples are 3D printed in two orthogonal build directions at various relative densities. Our results show that the work of fracture for octet lattices with build directions parallel to the crack plane is significantly higher than those with build directions perpendicular to the crack plane. We also observed that the ratio of specific work of fracture between the two build directions remains nearly constant across different relative densities. In contrast, the ratio of peak load between the two build directions decreases as relative density increases. Furthermore, the build direction dictates the fracture mechanism. While the perpendicular build direction predominantly results in a brittle (mode I) fracture, the parallel build direction leads to a complex, delamination-dominated (mode II type) fracture. This phenomenon is largely governed by the weak interfaces formed between the printed layers and their interaction with the lattice geometry. These results reveal that the build direction governs the fracture mechanism and work of fracture of these lattice metamaterials and is therefore an important design consideration.

3D printed PLA↗