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All sources NASA NTRS DOE OSTI

DOE OSTI2023

Enhanced Photoluminescence and Prolonged Carrier Lifetime through Laser Radiation Hardening and Self-Healing in Aged MAPbBr3 Perovskites Encapsulated in NiO Nanotubes

Organic-inorganic perovskites hold great promise as optoelectronic semiconductors for pure color light emitting and photovoltaic devices. However, challenges persist regarding their photostability and chemical stability, which limit their extensive applications. This paper investigates the laser radiation hardening and self-healing-induced properties of aged MAPbBr3 perovskites encapsulated in NiO nanotubes (MAPbBr3@NiO) using photoluminescence (PL) and fluorescence lifetime imaging (FLIM). After deliberately subjecting the MAPbBr3@ NiO to atmospheric conditions for two years, the sample remains remarkably stable. It exhibits no changes in PL wavelength during UV laser irradiation and self-healing. Furthermore, exposure to UV light at 375 nm enhances the PL of the self-healed MAPbBr3@NiO. FLIM analysis sheds light on the mechanism behind photodegradation, self-healing, and PL enhancement. The results indicate the involvement of many carrier-trapping states with low lifetime events and an increase in peak lifetime after self-healing. The formation of trapping states at the perovskite/nanotube interface is discussed and tested. This study provides new insights into the dynamics of photo-carriers during photodegradation and self-healing in organic-inorganic perovskites.

36 MATERIALS SCIENCE↗

DOE OSTI2023

The Role of Clay in Limiting Frictional Healing in Fault Gouges

Abstract Frictional healing is fundamental to the seismic cycle and plays a role in the energy balance, dynamics, and recurrence interval of earthquakes and slow slip events. Although the healing behavior of quartz has been studied extensively, the role of clay content is less understood. We tested synthetic mixtures of quartz and smectite (10%–100% smectite) in a double‐direct shear configuration to measure frictional healing. We show that the magnitude and rate of healing decreases systematically with higher clay content (from 0.008/decade at 10% smectite to 0.002/decade at 100% smectite). Healing scales with both the magnitude of stress relaxation during holds and layer‐normal compaction of the gouge. We suggest this reflects the alignment of clay minerals, leading to saturation of the real area of contact that limits restrengthening during holds. The low healing rates of clay‐rich faults—together with rate‐neutral to rate‐strengthening friction—should promote frequent, small failures or stable sliding.

58 GEOSCIENCES↗

NASA NTRS2011

Puncture Self-Healing Polymers for Aerospace Applications

Space exploration launch costs on the order of $10K per pound provide ample incentive to seek innovative, cost-effective ways to reduce structural mass without sacrificing safety and reliability. Damage-tolerant structural systems can provide a route to avoiding weight penalty while enhancing vehicle safety and reliability. Self-healing polymers capable of spontaneous puncture repair show great promise to mitigate potentially catastrophic damage from events such as micrometeoroid penetration. Effective self-repair requires these materials to heal instantaneously following projectile penetration while retaining structural integrity. Poly(ethylene-co-methacrylic acid) (EMMA), also known as Surlyn is an ionomer-based copolymer that undergoes puncture reversal (self-healing) following high impact puncture at high velocities. However EMMA is not a structural engineering polymer, and will not meet the demands of aerospace applications requiring self-healing engineering materials. Current efforts to identify candidate self-healing polymer materials for structural engineering systems are reported. Rheology, high speed thermography, and high speed video for self-healing semi-crystalline and amorphous polymers will be reported.

Gordon, Keith L.↗

DOE OSTI2022

Degradation and Self-Healing in Perovskite Solar Cells

Organic–inorganic halide perovskites are well-known for their unique self-healing ability. In the presence of strong external stimuli, such as light, temperature, and moisture, high-energy defects are created which can be healed by removing the perovskite from the degradation source. Furthermore, this self-healing ability has been showcased in devices with recoverable performance and day-and-night cycling operation to dramatically extend the device lifetime and even mechanical durability. However, to date, the mechanistic details and theory around this captivating trait are sparse and convoluted by the complex nature of perovskites. With a clear understanding of the intrinsic self-healing property, perovskite solar cells with extended lifetimes and durability can be designed to realize the large-scale commercialization of perovskite solar cells. Here, we spotlight the relevant degradation and self-healing literature and then propose design strategies to help conceptualize future research.

14 SOLAR ENERGY↗

DOE OSTI2023

Well-Tunable, 3D-printable, and Fast Autonomous Self-Healing Elastomers

Self-healing elastomers provide extended longevity of functional materials, due to their unique adaptability and durability. However, a major scientific challenge remains in developing materials with a rapid healing process combined with decent mechanical properties, that can be prepared by a relatively simple synthesis approach. Herein, we report a versatile design approach on self-healing elastomers by incorporating two different hydrogen bonding containing monomers, i.e., 2-[[(butylamino)carbonyl]oxy]ethyl acrylate (BCOE) and 2-ureido-4[1H]pyrimidinone (UPy) functionalized ethyl methacrylate. Poly(BCOE-r-UPy)s are synthesized by reversible addition-fragmentation chain-transfer (RAFT) polymerization, and controlling the ratio of two monomers enables well-tunable mechanical properties with tensile strength ranging from 0.04 to 6.3 MPa and tensile strain up to 3,000 %. The characteristic dissociation energy is calculated from a temperature dependence of terminal relaxation followed by subtracting the segmental relaxation. The rapid autonomous self-healing is achieved when the molar composition of Poly(BCOE-r-UPy) is tailored to BCOE/UPy = 99/1. The self-healing process is monitored in situ by a helium-ion microscope, and its macroscopic study using tensile tests indicates that Poly(BCOE-r-UPy1) with 1 % molar ratio of UPy recovers 70 % of its original toughness at ambient temperature within 10 mins. 3D printing of Poly(BCOE-r-UPy) affords a self-healable 3D structure, demonstrating the adaptability of Poly(BCOE-r-UPy) for on-demand fabrication. The simplicity of synthesis, well-tunable mechanical properties, unique self-healability, and 3D printing capability of Poly(BCOE-r-UPy)s indicate their potential for a range of applications.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Role of the Mineral in the Self-Healing of Cracks in Human Enamel

Human enamel is an incredibly resilient biological material, withstanding repeated daily stresses for decades. The mechanisms behind this resilience remain an open question, with recent studies demonstrating a crack-deflection mechanism contributing to enamel toughness and other studies detailing the roles of the organic matrix and remineralization. Here, we focus on the mineral and hypothesize that self-healing of cracks in enamel nanocrystals may be an additional mechanism acting to prevent catastrophic failure. To test this hypothesis, we used a molecular dynamics (MD) approach to compare the fracture behavior of hydroxyapatite (HAP) and calcite, the main minerals in human enamel and sea urchin teeth, respectively. In this work, we find that cracks heal under pressures typical of mastication by fusion of crystals in HAP but not in calcite, which is consistent with the resilience of HAP enamel that calcite teeth lack. Scanning transmission electron microscopy (STEM) images of structurally intact ("sound") human enamel show dashed-line nanocracks that resemble and therefore might be the cracks healed by fusion of crystals produced in silico . The fast, self-healing mechanism shown here is common in soft materials and ceramics but has not been observed in single crystalline materials at room temperature. The crack self-healing in sound enamel nanocrystals, therefore, is unique in the human body and unique in materials science, with potential applications in designing bioinspired materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2003

Hindlimb unloading alters ligament healing

We investigated the hypothesis that hindlimb unloading inhibits healing in fibrous connective tissue such as ligament. Male rats were assigned to 3- and 7-wk treatment groups with three subgroups each: sham control, ambulatory healing, and hindlimb-suspended healing. Ambulatory and suspended animals underwent surgical rupture of their medial collateral ligaments, whereas sham surgeries were performed on control animals. After 3 or 7 wk, mechanical and/or morphological properties were measured in ligament, muscle, and bone. During mechanical testing, most suspended ligaments failed in the scar region, indicating the greatest impairment was to ligament and not to bone-ligament insertion. Ligament testing revealed significant reductions in maximum force, ultimate stress, elastic modulus, and low-load properties in suspended animals. In addition, femoral mineral density, femoral strength, gastrocnemius mass, and tibialis anterior mass were significantly reduced. Microscopy revealed abnormal scar formation and cell distribution in suspended ligaments with extracellular matrix discontinuities and voids between misaligned, but well-formed, collagen fiber bundles. Hence, stress levels from ambulation appear unnecessary for formation of fiber bundles yet required for collagen to form structurally competent continuous fibers. Results support our hypothesis that hindlimb unloading impairs healing of fibrous connective tissue. In addition, this study provides compelling morphological evidence explaining the altered structure-function relationship in load-deprived healing connective tissue.

NASA Discipline Musculoskeletal↗

NASA NTRS2017

Self-Healing Technologies for Wiring and Surfaces in Aerospace and Deep Space Exploration Applications

Self-healing technologies have been identified as critical technology gaps for future exploration. NASA and KSC have been working in this area for multiple years with established intellectual property; however, there are many challenges that remain in this area of research. How do we mimic what the body does so naturally when we as NASA have unique requirements? We have been investigating several mechanisms for self-healing: microencapsulation with a healant core to fill in voids in the case of mechanical puncture and flowable (or sealable)systems that have inherent chemical properties that allow the materials to flow back together when cut or damaged. The microcapsules containing healant have to be durable and robust, must be able to take high temperatures to meet NASA unique requirements, provide good capillary flow of the healant, and be small in diameters to fill in damage voids in thin films or surfaces. Sealable systems have to flow in a range of temperatures and yet be lightweight and chemically resistant. The systems currently being developed are based on polyimide and polyurethane matrices and have been studied for use in high performance wiring systems, inflatable systems, and habitation structures. Self-healing or self-sealing capability would significantly reduce maintenance requirements and increase the safety and reliability performance of critical systems. Advances in these self-healing technologies and some of the unique challenges needed to be overcome in order to incorporate a self-healing mechanism into wiring or thin films systems will be addressed.

Self-healing technologies↗

DOE OSTI2021

Progress and Challenges in Self-Healing Cementitious Materials

Concrete is the most used man-made material today consisting of a mixture of aggregates (sand, gravel, crashed rock) and paste. The paste component, made up of cement and water, cracks with time. Despite this shortcoming, research towards next-generation cement and concrete has only taken a boost in the past 10-15 years. In particular, self-healing cementitious materials is a research area that has attracted a great deal of attention. A number of reported novel formulations have demonstrated an increase in mechanical and chemical stability with respect to conventional Portland cement, through the addition of inorganic, organic, and even biological additives. This review reports on the latest advances in cement research related to the synthesis of self-healing cements applied in concrete structures. These include geopolymers, engineered cementitious materials (ECC), bacterial cement composites, microencapsulated self-healing materials, shape memory alloys (SMA), and polymer-cement composites. This work describes the performance of each cementitious material and the mechanism responsible for self-healing, including a section on the latest computational modeling studies towards this end. A detailed understanding of these various self-healing cement technologies, including their strengths and weaknesses, is critical at the time of determining the type of structures that these materials could be used for.

Fernandez, Carlos A.↗

DOE OSTI2020

Water accelerated self-healing of hydrophobic copolymers

Previous studies have shown that copolymer compositions can significantly impact self-healing properties. This was accomplished by enhancement of van der Waals (vdW) forces which facilitate self-healing in relatively narrow copolymer compositional range. In this work we report the acceleration of self-healing in alternating/random hydrophobic acrylic-based copolymers in the presence of confined water molecules. Under these conditions competing vdW interactions do not allow H 2 O-diester H-bonding, thus forcing nBA side groups to adapt L-shape conformations, generating stronger dipole-dipole interactions resulting in shorter inter-chain distances compared to ‘key-and-lock’ associations without water. The perturbation of vdW forces upon mechanical damage in the presence of controllable amount of confined water is energetically unfavorable leading the enhancement of self-healing efficiency of hydrophobic copolymers by a factor of three. The concept may be applicable to other self-healing mechanisms involving reversible covalent bonding, supramolecular chemistry, or polymers with phase-separated morphologies.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Non-disruptive error field identification based on magnetic island healing

Here a technique to identify intrinsic error fields (EFs) in tokamaks with minimized risk of disruption is demonstrated on the DIII-D tokamak. The method extends the conventional driven magnetic island ‘compass scan’ approach by modifying asynchronous control waveforms to enable prompt healing of the island instability. Healing of the island is achieved by reducing the imposed non-axisymmetric coil current and raising the density (here via gas fueling). The method is also shown to support multiple island threshold measurements per pulse, thus reducing the number of dedicated pulses necessary to conduct an EF identification. Non-linear modeling with the TM1 code reproduces the experimental results and approximately recovers the critical density required for island healing. Island healing is explained in the non-linear modeling by an increase in the viscous coupling between the static island and the nearby flowing plasma, thus healing the island as it accelerates into the plasma frame. Due to both simplicity and risk minimization, this technique is suitable for plasma-based EF identification in the early commissioning stages of future disruption-averse tokamaks such as ITER and SPARC.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

A recyclable self-healing composite with advanced sensing property

Polymer-based composites frequently encounter damage, often lurking beneath the surface and proving challenges to their early detection and repair. While material-based sensors show promise for encoding self-sensing properties within these composites, their in situ healing and reprocessability remain significant challenges. Therefore, the overarching goal of this study is the creation of a reprocessable polymeric composite encoded with self-healing attributes and the ability to autonomously sense damage. At the core of this innovation are vitrimers, a polymeric material characterized by a covalently adaptive dynamic network responsive to external factors such as heat. They combine thermoset-like resilience with thermoplastic-like flowability on demand under external stimuli. We nanoengineer a polyester-based vitrimeric polymer by incorporating piezoresistive carbon nanotubes (CNTs) as reinforcing elements that not only enhance its mechanical strength but also create a percolation network within the composite, thereby enabling piezoresistive self-sensing properties, all the while preserving the intrinsic self-healing capabilities offered by the vitrimeric matrix. The fabrication process of the composite involves a solvent-free in situ polymerization method that combines epoxy and anhydride-containing monomers with ~ 0.1 wt.% of CNTs. Once it was established that the introduction of CNTs into the polymeric matrix did not compromise the mechanical properties of the composite, their strain-sensing properties were characterized by applying cyclic loading while measuring their electrical resistance. Strikingly, CNT-enhanced vitrimer composite consistently retains its mechanical and sensing properties through repeated cycles of reshaping and reprocessing, underscoring its potential as a robust distributed strain sensor. This polyester-based vitrimeric composite is also easily recyclable without harsh chemical treatments. Preliminary findings from this study conclusively demonstrate that the bulk composite boasts both self-sensing capabilities and in situ detect healing properties, charting a promising course towards the development of a mechanically resilient multifunctional composite that seamlessly integrates selfsensing and healing capabilities.

Rohewal, Sargun Singh↗

DOE OSTI2021

Dual Function Solid State Battery with Self-Forming Self-Healing Electrolyte and Separator (Final Scientific/Technical Report)

Over the course of this program, we have demonstrated an improved rechargeable Li/I2 battery with reduced impedance, improved cyclability, improved Coulombic Efficiency, and the ability to “self-heal” during shorting events. Multi-year efforts have led to the development and improvements in the composition, fabrication, and preparation of the solid state electrolyte, the role of the interface, and design of appropriate test conditions. These investigations have led to significant improvements in Coulombic efficiency. By systematic development of a composite solid state electrolyte, this system is able to self-form upon charge, thus lending itself to long shelf life before use. The initial project objective was to demonstrate a solid-state rechargeable battery based on a Li-metal anode and iodine cathode with a self-forming, self-healing electrolyte and separator with high gravimetric and volumetric energy density. The final deliverables of this project build on a multi-year effort beginning with materials development and design to generate a suitable solid state electrolyte composite with demonstrated higher ionic conductivity compared to the baseline (LiI). Development in cell design and interface modification leading to the generation of rechargeable solid electrolyte cells with Coulombic efficiency improvements of ~3X over initial tests, as well as demonstration of self-healing behavior, where the cells retained their ability to continue extended cycling after shorting events. The hypothesis put forward as part of the initial concept for the project was that the cell chemistry would be self-healing. For example, if a lithium dendrite formed during charge of the cell and reached the iodine cathode, the reaction of the lithium dendrite with the iodine would consume the tip of the dendrite to form lithium iodide, more of the solid electrolyte. The formation of the solid electrolyte would allow the cell to recover and continue to function. This type of self-healing during cycling has been demonstrated and has the potential to improve on safety considerations that stem from shorting events in other Li- containing systems.

25 ENERGY STORAGE↗

NASA NTRS2011

Microencapsulation of Self Healing Agents for Corrosion Control Coatings

Corrosion, the environmentally induced degradation of materials, is a very costly problem that has a major impact on the global economy. Results from a 2-year breakthrough study released in 2002 by the U.S. Federal Highway Administration (FHWA) showed that the total annual estimated direct cost associated with metallic corrosion in nearly every U.S. industry sector was a staggering $276 billion, approximately 3.1% of the nation's Gross Domestic Product (GOP). Corrosion protective coatings are widely used to protect metallic structures from the detrimental effects of corrosion but their effectiveness can be seriously compromised by mechanical damage, such as a scratch, that exposes the metallic substrate. The incorporation of a self healing mechanism into a corrosion control coating would have the potential to significantly increase its effectiveness and useful lifetime. This paper describes work performed to incorporate a number of microcapsule-based self healing systems into corrosion control coatings. The work includes the preparation and evaluation of self-healing systems based on curable epoxy, acrylate, and siloxane resins, as well as, microencapsulated systems based on passive, solvent born, healing agent delivery. The synthesis and optimization of microcapsule-based self healing systems for thin coating (less than 100 micron) will be presented.

Jolley, S. T.↗

DOE OSTI2023

A Self‐Healing Chemistry‐Enabled Organic Cathode for Sustainable and Stable Sodium‐Ion Batteries

Sodium‐on batteries (SIBs) are promising alternatives to lithium‐ion batteries (LIBs) because of the low cost, abundance, and high sustainability of sodium resources. Analogous to LIBs, the high‐capacity electrodes in SIBs always suffer from rapid capacity decay upon long‐term cycling due to the particle pulverization induced by a large volume change. Circumventing particle pulverization plays a critical role in developing high‐energy and long‐life SIBs. Herein, tetrahydroxy‐1,4‐benzoquinone disodium salt (TBDS) that can self‐heal the cracks by hydrogen bonding between hydroxyl group and carbonyl group is employed as a cathode for sustainable and stable SIBs. The self‐healing TBDS exhibits long cycle life of 1000 cycles with a high rate capability up to 2 A g −1 due to the fast Na‐ion diffusion reaction in the TBDS cathode. The intermolecular hydrogen bonding has been comprehensively characterized to understand the self‐healing mechanism. The hydrogen bonding‐enabled self‐healing organic materials are promising for developing high‐energy and long‐cycle‐life SIBs.

25 ENERGY STORAGE↗

DOE OSTI2025

Confinement-Driven Segregation Enables Glassy Polymer Hybrid Materials Featuring Disordered Hyperuniformity and Integrated Self-Healing

The blending of glassy copolymer-brush modified colloids with a viscoelastic linear copolymer featuring intrinsic self-healing enabled disordered hyperuniform hybrid materials that combined mechanical robustness with structural color, processability, environmental stability, and the ability to recover structure and properties after incurring physical damage via ‘integrated self-healing’. Symmetric linear n-butyl acrylate/methyl methacrylate (BA/MMA) were co-assembled with asymmetric glassy BA/MMA statistical copolymer brush (silica) particles. ‘Confinement-driven segregation’ resulted in a microphase-separated morphology in which the linear copolymer resided within the interstitial regions of a rigid (∼1 GPa) copolymer brush particle template with disordered hyperuniform microstructure. Diffusion of the self-healing copolymer additive into damage regions drove the recovery after damage, along with the restoration of structural color due to the materials hyperuniform microstructure. The synergistic action of intrinsic and extrinsic healing mechanisms could provide a versatile platform for the bottom-up fabrication of multifunctional hybrid materials with increased damage resistance and functional longevity.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Self-Healing Lithium Dendrites through Spontaneous Passivating Layer Formation for Stable Solid-State Lithium–Metal Batteries

All-solid-state lithium–metal batteries have attracted significant attention, owing to their high energy density and superior safety. However, lithium–metal penetration through the solid electrolyte, leading to short-circuiting, remains a critical failure mode that demands comprehensive mitigation strategies. Most existing strategies are effective only prior to the initiation of lithium-dendrite formation and fail once dendrites begin to propagate through the electrolyte. In this study, we propose a self-healing mechanism in which the penetrated lithium reacts with a self-healing agent to form a passivating layer along the particle boundaries. Lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) was incorporated into a Li 6 PS 5 Cl solid electrolyte as the self-healing agent to suppress lithium-dendrite propagation even after dendrite formation initiated under high current densities. The self-healing induced by LiTFSI was verified through comprehensive experimental analyses and was further demonstrated in a full-cell configuration. Moreover, LiTFSI incorporation plays an important role in increasing the critical current density by reducing the overall electronic conductivity of the solid electrolyte and facilitating the formation of a robust LiF-containing solid-electrolyte interphase.

25 ENERGY STORAGE↗

DOE OSTI2021

Age-associated expression of p21and p53 during human wound healing

In mice, cellular senescence and senescence-associated secretory phenotype (SASP) positively contribute to cutaneous wound healing. In this proof-of-concept study, we investigated the expressions of p16, p21, and other senescence-associated biomarkers during human wound healing in 24 healthy subjects using a double-biopsy experimental design. The first punch biopsy created the wound and established the baseline. The second biopsy, concentric to the first and taken several days after wounding, was used to probe for expression of biomarkers by immunohistochemistry and RNA FISH. To assess the effects of age, we recruited 12 sex-matched younger (30.2 ± 1.3 years) and 12 sex-matched older (75.6 ± 1.8 years) subjects. We found that p21 and p53, but not p16, were induced during healing in younger, but not older subjects. A role for Notch signaling in p21 expression was inferred from the inducible activation of HES1. Further, other SASP biomarkers such as dipeptidyl peptidase-4 (DPP4) were significantly induced upon wounding in both younger and older groups, whereas matrix metallopeptidase 9 (MMP9) was induced only in the younger group. Senescence-associated β-galactosidase (SA-β-gal) was not detectable before or after wounding. This pilot study suggests the possibility that human cutaneous wound healing is characterized by differential expression of p21 and p53 between younger and older subjects.

59 BASIC BIOLOGICAL SCIENCES↗