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DOE OSTI2024

A Self-Healing, Flowable, Yet Solid Electrolyte Suppresses Li-Metal Morphological Instabilities

In this article, lithium metal (Li 0 ) solid-state batteries encounter implementation challenges due to dendrite formation, side reactions, and movement of the electrode–electrolyte interface in cycling. Notably, voids and cracks formed during battery fabrication/operation are hot spots for failure. Here, a self-healing, flowable yet solid electrolyte composed of mobile ceramic crystals embedded in a reconfigurable polymer network is reported. This electrolyte can auto-repair voids and cracks through a two-step self-healing process that occurs at a fast rate of 5.6 µm h -1 . A dynamical phase diagram is generated, showing the material can switch between liquid and solid forms in response to external strain rates. The flowability of the electrolyte allows it to accommodate the electrode volume change during Li 0 stripping. Simultaneously, the electrolyte maintains a solid form with high tensile strength (0.28 MPa), facilitating the regulation of mossy Li 0 deposition. The chemistries and kinetics are studied by operando synchrotron X-ray and in situ transmission electron microscopy (TEM). Solid-state NMR reveals a dual-phase ion conduction pathway and rapid Li + diffusion through the stable polymer-ceramic interphase. This designed electrolyte exhibits extended cycling life in Li 0 –Li 0 cells, reaching 12 000 h at 0.2 mA cm -2 and 5000 h at 0.5 mA cm -2 . Furthermore, owing to its high critical current density of 9 mA cm -2 , the Li 0 –LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) full cell demonstrates stable cycling at 5 mA cm -2 for 1100 cycles, retaining 88% of its capacity, even under near-zero stack pressure conditions.

25 ENERGY STORAGE↗

DOE OSTI2022

A Bioinspired Artificial Injury Response System Based on a Robust Polymer Memristor to Mimic a Sense of Pain, Sign of Injury, and Healing

Abstract Flexible electronic skin with features that include sensing, processing, and responding to stimuli have transformed human–robot interactions. However, more advanced capabilities, such as human‐like self‐protection modalities with a sense of pain, sign of injury, and healing, are more challenging. Herein, a novel, flexible, and robust diffusive memristor based on a copolymer of chlorotrifluoroethylene and vinylidene fluoride (FK‐800) as an artificial nociceptor (pain sensor) is reported. Devices composed of Ag/FK‐800/Pt have outstanding switching endurance >10 6 cycles, orders of magnitude higher than any other two‐terminal polymer/organic memristors in literature (typically 10 2 –10 3 cycles). In situ conductive atomic force microscopy is employed to dynamically switch individual filaments, which demonstrates that conductive filaments correlate with polymer grain boundaries and FK‐800 has superior morphological stability under repeated switching cycles. It is hypothesized that the high thermal stability and high elasticity of FK‐800 contribute to the stability under local Joule heating associated with electrical switching. To mimic biological nociceptors, four signature nociceptive characteristics are demonstrated: threshold triggering, no adaptation, relaxation, and sensitization. Lastly, by integrating a triboelectric generator (artificial mechanoreceptor), memristor (artificial nociceptor), and light emitting diode (artificial bruise), the first bioinspired injury response system capable of sensing pain, showing signs of injury, and healing, is demonstrated.

36 MATERIALS SCIENCE↗

DOE OSTI2024

In Situ Alloying Enabled by Active Liquid Metal Filler for Self‐Healing Composite Polymer Electrolytes

Abstract Solid inorganics, known for kinetically inhibiting polymer crystallization and enhancing ionic conductivity, have attracted significant attention in solid polymer electrolytes. However, current composite polymer electrolytes (CPEs) are still facing challenges in Li metal batteries, falling short of inhibiting severe dendritic growth and resulting in very limited cycling life. This study introduces Ga 62.5 In 21.5 Sn 16 (Galinstan) liquid metal (LM) as an active liquid alternative to conventional passive solid fillers, aiming at realizing self‐healing protection against dendrite problems. Compared to solid inorganics, for example silica, LM droplets could more significantly reduce polymer crystallinity and enhance Li‐ion conductivity due to their liquid nature, especially at temperatures below the polymer melting point. More importantly, LMs are unraveled as dynamic chemical traps, which are capable of blocking and consuming lithium dendrites upon contact via in situ alloying during battery operation and further inhibiting dendritic growth due to the lower deposition energy barrier of the formed Li‐LM alloy. As a proof of concept, by strategically designing an asymmetric CPE with the active LM filling, a solid‐state Li/LiFePO 4 battery achieves promising full‐cell functionality with notable rate performance and stable cycle life. This active filler‐mediated self‐healing approach could bring new insights into the battery design in versatile solid‐state systems.

Wu, Kai↗

DOE OSTI2020

Mechanical and self-healing behavior of low carbon engineered cementitious composites reinforced with PP-fibers

While the ultrahigh tensile ductility and superior durability of Engineered Cementitious Composites (ECC) have been demonstrated, the relatively high energy and carbon intensity, as well as high material cost present potential impediments to broader ECC applications. The objective of this research is to develop a more sustainable and cost-effective ECC. The ordinary Portland cement (OPC) and the commonly used PVA fiber in conventional ECC were replaced by limestone calcined clay cement (LC3) and polypropylene (PP) fiber, respectively. The ECC compressive strength, tensile stress-strain relationship, and microcrack self-healing behavior were studied at three water to binder ratios (0.3, 0.2, 0.16). The novel LC3-PP-ECC showed a tensile strain capacity of greater than 6% and an intrinsically tight crack width below 82 μm when loaded to 1% tensile strain. Further, the LC3-PP-ECC demonstrated efficient recovery of the composite tensile ductility and ultimate tensile strength through self-healing. Compared to typical ECC made with OPC and PVA fiber, the material cost, embodied energy and carbon footprint of LC3-PP-ECC are reduced by 61%, 45%, and 48%, respectively. Here, the superior mechanical properties and durability combined with the low environmental impact and cost for material production promote LC3-PP-ECC as a sustainable material for structural and non-structural applications.

42 ENGINEERING↗

DOE OSTI2025

Recent Warming of the Southern Hemisphere Subtropical Lower Stratosphere and Antarctic Ozone Healing

Observed temperature changes from 2002 to 2022 reveal a pronounced warming of the Southern Hemisphere (SH) subtropical lower stratosphere, and a cooling of the Antarctic lower stratosphere. In contrast, model simulations of 21st-century stratospheric temperature changes show widespread cooling driven by increasing greenhouse gases, with local warming in the Antarctic lower stratosphere due to ozone healing. We provide evidence that these discrepancies between observed and simulated stratospheric temperature changes are linked to a slowdown of the Brewer-Dobson Circulation, particularly in the SH. These changes in the stratospheric circulation are strongest from October through December. This altered circulation warms the SH subtropical lower stratosphere while cooling the Antarctic lower stratosphere, canceling and even reversing the Antarctic ozone recovery that would have occurred in its absence during this period. When circulation changes are accounted for, the SH subtropical lower-stratospheric warming is removed, and Antarctic lower-stratospheric warming is revealed with enhanced ozone healing, highlighting the crucial role of the stratospheric circulation in shaping temperature and ozone changes.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

Self-healing oxygen evolution catalysts

Abstract Electrochemical and photoelectrochemical water splitting offers a scalable approach to producing hydrogen from renewable sources for sustainable energy storage. Depending on the applications, oxygen evolution catalysts (OECs) may perform water splitting under a variety of conditions. However, low stability and/or activity present challenges to the design of OECs, prompting the design of self-healing OECs composed of earth-abundant first-row transition metal oxides. The concept of self-healing catalysis offers a new tool to be employed in the design of stable and functionally active OECs under operating conditions ranging from acidic to basic solutions and from a variety of water sources.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Self-healing magnetic nanocomposites with robust mechanical properties and high magnetic actuation potential prepared from commodity monomers via graft-from approach

Herein, we report the design, synthesis and characterization of self-healing magnetic nanocomposites prepared from readily available commodity monomers. These multi-functional materials demonstrate robust mechanical properties, with a Young's modulus of 70 MPa and over 500% extensibility. The magnetic nanocomposites also show self-healing ability, achieving 46% recovery of extensibility in 5 hours in ambient conditions while retaining high magnetic actuation with a commodity magnet.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Enhanced stability of silicon for photoelectrochemical water oxidation through self-healing enabled by an alkaline protective electrolyte

Alkaline electrolytes impede the corrosion of Si photoanodes under positive potentials and/or illumination, due to the formation of a SiO x layer that etches 2–3 orders of magnitude more slowly than Si. Hence during water oxidation under illumination, pinholes in protection layers on Si photoanodes result in the local formation of a protective, stabilizing passive oxide on the Si surface. However, operation under natural diurnal insolation cycles additionally requires protection strategies that minimize the dark corrosive etching rate of Si at pinholes. We show herein that addition of [Fe(CN) 6 ] 3- to 1.0 M KOH(aq) results in a self-healing process that extends the lifetime to >280 h of an np + -Si(100) photoanode patterned with an array of Ni catalyst islands operated under simulated day/night cycles. The self-healing [Fe(CN) 6 ] 3- additive caused the exposed Si(100) surface to etch >180 times slower than the Si etch rate in 1.0 M KOH(aq) alone. No appreciable difference in etch rate or facet preference was observed between Si(100) and Si(111) surfaces in 1.0 M KOH(aq) with [Fe(CN) 6 ] 3- , indicating that the surface conformally oxidized before Si dissolved. The presence of [Fe(CN) 6 ] 3- minimally impacted the faradaic efficiency or overpotential of p + -Si/Ni electrodes for the oxygen-evolution reaction.

25 ENERGY STORAGE↗

DOE OSTI2021

Integrating Transactive Energy into Reliability Evaluation for a Self-healing Distribution System with Microgrid

Non-utility owned distributed energy resources (DERs) are mostly untapped currently, but they can provide many grid services such as voltage regulation and service restoration, if properly controlled, and can improve the distribution systems reliability when coordinated with utility-owned assets such as self-healing control and microgrids. This paper integrates transactive energy control into the distribution system reliability evaluation to quantitatively assess the impact of non-utility owned DERs on reliability improvement. Here, a transactive reactive power control strategy is designed to incentivize the DERs to provide reactive power support for improving voltage profiles thus enabling additional customer load restoration during an outage. Also, an operational sequence to coordinate the non-utility owned DERs with the utility owned self-healing control and utility owned microgrids is designed and integrated into the service restoration process with the operational constraints guaranteed by checking the three-phase unbalanced power flow for post-fault network reconfiguration. The reliability indices are then calculated through a Monte Carlo simulation. The transactive reactive power control strategy is tested on a four-feeder distribution system operated by Duke Energy in the U.S. Results demonstrate that the non-utility owned DERs with the transactive control improve the reliability of both the system and critical loads by more than 30%.

24 POWER TRANSMISSION AND DISTRIBUTION↗

DOE OSTI2023

AmeriFlux FLUXNET-1F US-xHE NEON Healy (HEAL)

This is the AmeriFlux Management Project (AMP) created FLUXNET-1F version of the carbon flux data for the site US-xHE NEON Healy (HEAL). This is the FLUXNET version of the carbon flux data for the site US-xHE NEON Healy (HEAL) produced by applying the standard ONEFlux (1F) software.

Network), NEON (National Ecological Observatory↗

DOE OSTI2021

Self-Healing Ceramics and Mechanical Metamaterials

We performed large scale molecular dynamics (MD) simulations and reactive & quantum molecular dynamics simulations to investigate: (1) faceting, grain growth, and crack healing in ceramics; (2) stress-release mechanism and healing in fibers; and (3) mechanical properties of two-dimensional metamaterials. We also designed highly accurate interatomic potentials and forces using artificial neural networks (ANN) and first-principles molecular dynamics simulation data for use in our MD and reactive MD simulations. We demonstrated the efficacy of modeling quantum materials atomistic simulation data using unsupervised deep learning approaches on a quantum computer. These achievements are elaborated in the following sections.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Self-Healing Polymer-Modified Cements for Ambient-Temperature Applications

We present two novel polymer-modified cement formulations which can self-heal cement microfractures at ambient temperature. The polymers used are either commercially available boric acid gel (BAG) or a synthesized polymer MBA-BDA. This report summarizes the progress of developing polymer-modified cement formulations. The polymers used are either commercially available or synthesized in house. Results show two formulations (commercial boric acid gel BAG and as-synthesized polymer MBA-BDA), both with potential to bring about room-temperature self-healing to conventional cement.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Synthesis of multiphase self-healing polymers from commodity monomers

A self-healing polymer material that includes a multiphase copolymer, and a method of making the copolymer, are provided. The multiphase copolymer includes one or more hydrogen bond-forming copolymer segments, each segment including a polymerized acrylamide monomer and a polymerized acrylic monomer. The polymerized acrylamide monomer includes functional groups that form hydrogen bonds in the multiphase copolymer, and is present in the one or more copolymer segments in an amount sufficient for self-healing of the multiphase copolymer.

Guan, Zhibin↗

DOE OSTI2022

Self-healing barrier films for vacuum insulation panels

A self-healing vacuum insulation panel and a method of manufacture are provided. The vacuum insulation panel includes a self-healing, multi-layer barrier film including a separator between a curing agent and a curable resin. Upon damage to the separator, the curing agent penetrates the separator due to a pressure differential across the barrier film and reacts with the curable resin to seal any cuts or punctures. The curing agent and the curable resin can be selected to have long term stability and a short reaction time with no need for external stimuli. As a result, the multi-layer barrier film can retain the internal vacuum and maintain a desirably low thermal conductivity using low-cost, commercially available epoxies and curing agents.

Biswas, Kaushik↗

DOE OSTI2024

Self-healing macromolecular crystal materials

Hybrid materials are disclosed including molecular/protein crystals integrated with synthetic polymers. The disclosed materials combine the structural order and periodicity of crystals, the adaptiveness and tunable mechanical properties of polymeric networks, and the chemical versatility of protein building blocks. Some of the properties of the disclosed materials include the following: 1) allows crystals—which are typically rigid and brittle—to expand and contract reversibly; 2) incorporates polymers to increase the mechanical toughness of the crystals and allow self-healing; 3) reversibly expand/contract crystal lattices and mobilize the protein components therein may provide a new means to improve X-ray diffraction quality and explore otherwise inaccessible protein structural states using 3D protein crystallography; 4) creation of chemically and mechanically differentiated domains within single crystals. Some example embodiments combine the properties of hydrogels (flexibility, adaptability, elasticity, self-healing), crystals (structural order) and proteins (chemical and genetic tailorability).

Tezcan, Faik↗

DOE OSTI2023

Structure, Function, and Application of Self–Healing Adhesives from Mistletoe Viscin

Berries from the European Mistletoe (Viscum album) possess a sticky tissue called viscin that facilitates adhesion and germination onto host trees. Recent studies of viscin have demonstrated its adhesive capacity on a range of natural and synthetic surfaces including wood, skin, metals, and plastic. Yet, the underlying mechanisms remain poorly understood. Here, an investigation of the adhesive performance of mistletoe viscin is performed, demonstrating its hygroscopic nature and ability to self-heal following adhesive failure. It is identified that adhesion originates from a water-soluble adhesive component that can be extracted, isolated, and characterized independently. Lap shear mechanical testing indicates that the mistletoe adhesive extract (MAE) outperforms native viscin tissue, as well as gum arabic and arabinogalactan—common plant-based adhesives. Furthermore, humidity uptake experiments reveal that MAE can reversibly absorb nearly 100% of its mass in water from the atmosphere. In-depth spectroscopic and mass spectrometry investigations reveal a composition consisting primarily of an atypical arabinogalactan, with additional sugar alcohols. Finally, several proof-of-concept applications are demonstrated using MAE for hygro-responsive reversible adhesion between various surfaces including skin, plastic, PDMS, and paper, revealing that MAE holds potential as a biorenewable and reusable adhesive for applications in cosmetics, packaging, and potentially, tissue engineering.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Intrinsic property of defective β-Ga 2 O 3 to self-heal under ionizing irradiation

Damage evolution and phase stability in defective β-Ga 2 O 3 and an irradiation-converted γ-Ga 2 O 3 layer have been studied under ionizing irradiation at 300 K. By exploring athermal nonequilibrium processes in β-Ga 2 O 3 , we succeed in identifying a self-healing mechanism that enables recovery pre-existing damage, characterized by a recovery cross-section of ~0.17 nm 2 . Remarkably, this study further demonstrates that the crystallinity of the irradiation-converted γ-Ga 2 O 3 layer improves under ionizing irradiation. More importantly, X-ray diffraction analysis reveals that the highly-strained 𝛾 -phase transforms into a highly-crystalline structure without film disintegration, contrasting to that reported for isochronal annealing at 1000 K. The inelastic thermal spike calculations provide insights into the important effects of energy transfer to electrons in reordering the local atomic arrangement of both defective β- Ga 2 O 3 and 𝛾-Ga 2 O 3 . This behavior suggests a pathway for low-temperature crystallization, offering a promising strategy for fabricating ultrahigh-speed non-volatile memory devices.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Robust Self-Healing Adhesives Based on Dynamic Urethane Exchange Reactions

Thermoset polyurethanes (PUs) have been successfully reprocessed as covalent adaptable networks (CANs) by catalyzing carbamate exchange. Here we extend bond exchange beyond the internal network cross-links to create a dynamic urethane adhesive. Interfacing PU CANs to substrates with nucleophilic functional groups creates adhesives capable of reversible transcarbamoylation with the substrate, which has not been demonstrated previously by CAN adhesives. Two types of thermoset PU films were synthesized, one containing the green carbamate exchange catalyst Zr(tmhd)4 and the other containing no catalyst. Although otherwise identical in chemical and network properties, as indicated by FT-IR spectroscopy and dynamic mechanical thermal analysis (DMTA), the film containing catalyst showed dynamic bond exchange behavior through stress relaxation analysis. When evaluated as an adhesive, the CAN film exhibited self-healing properties and retained its adhesive strength for five cycles, which is attributed to reversible covalent bonding to the glass substrate. Furthermore, this work expands industrially relevant CANs to structural adhesives and demonstrates their potential value in an application that presently employs PUs as single-use materials.

adhesive↗