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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Zeolitic Imidazole Framework Decorated Substrates for Lead Removal From Water

Lead contamination in water supplies necessitates efficient and mechanistically understood removal strategies. Zeolitic imidazole frameworks (ZIFs) are promising adsorbents; however, ZIF-67 (Co-based) is more susceptible to hydrolysis than its zinc analogue ZIF-8, raising questions about stability during metal uptake. In this study, we systematically compare ZIF-8 and ZIF-67 under controlled pH conditions and evaluate how substrate anchoring influences hydrolytic stability and Pb 2+ adsorption behavior. By integrating adsorption capacity measurements, kinetic analysis, metal-node leaching data, and structural characterization, we distinguish ion exchange from framework degradation and clarify the temporal interplay between adsorption and hydrolysis. Although ZIF-67 exhibits greater hydrolytic sensitivity, coordination with phosphoryl-bearing Mucor hiemalis membranes significantly reduces Co 2+ leaching and enhances structural retention. Under the optimized conditions (pH 5), ZIF-67@Mucor achieves a maximum Pb 2+ adsorption capacity of 867 mg g −1 . These findings demonstrate that substrate-dependent stabilization enables controlled exploitation of ZIF reactivity for aqueous metal remediation.

Adsorption↗
DOE OSTI2025

A plant-specific cytochrome b 5 –like protein is essential for phytosterol biosynthesis

Sterols are essential isoprenoid derivatives that contribute to membrane structure and function. In plants, they also serve as precursors to phytohormones and specialized metabolites important for development, defense, and health. Although the sterol biosynthetic pathway is considered well-characterized, we report the discovery of a plant-specific cytochrome b 5 –like protein, CB5LP, as a critical component of phytosterol biosynthesis. Loss of CB5LP in Arabidopsis causes embryonic defects, seedling lethality, and accumulation of 14α-methyl-sterols, with reduced levels of sitosterol and stigmasterol—indicating a defect in sterol 14α-demethylation. TurboID-based proximity labeling and in vitro assays show that CB5LP physically and functionally interacts with CYP51, a cytochrome P450 enzyme catalyzing this demethylation step. Unlike canonical cytochrome b 5 proteins, CB5LP has a reversed topology and is exclusive to plants, acting as an evolutionarily distinct electron donor. This discovery reveals an uncharacterized redox partnership essential for sterol biosynthesis and highlights a promising target for the development of selective herbicide.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Cell-Free Screening, Production and Animal Testing of a STI-Related Chlamydial Major Outer Membrane Protein Supported in Nanolipoproteins

Background: Vaccine development against Chlamydia, a prevalent sexually transmied infection (STI), is imperative due to its global public health impact. However, significant challenges arise in the production of effective subunit vaccines based on recombinant protein antigens, particularly with membrane proteins like the Major Outer Membrane Protein (MOMP). Methods: Cellfree protein synthesis (CFPS) technology is an aractive approach to address these challenges as a method of high-throughput membrane protein and protein complex production coupled with nanolipoprotein particles (NLPs). NLPs provide a supporting scaffold while allowing easy adjuvant addition during formulation. Over the last decade, we have been working toward the production and characterization of MOMP-NLP complexes for vaccine testing. Results: The work presented here highlights the expression and biophysical analyses, including transmission electron microscopy (TEM) and dynamic light scaering (DLS), which confirm the formation and functionality of MOMP-NLP complexes for use in animal studies. Moreover, immunization studies in preclinical models compare the past and present protective efficacy of MOMP-NLP formulations, particularly when co-adjuvanted with CpG and FSL1. Conclusion: Ex vivo assessments further highlight the immunomodulatory effects of MOMP-NLP vaccinations, emphasizing their potential to elicitrobust immune responses. However, further research is warranted to optimize vaccine formulations further, validate efficacy against Chlamydia trachomatis, and beer understand the underlying mechanisms of immune response.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2025

Rippled metamaterials with scale-dependent tailorable elasticity

Thermally induced ripples are intrinsic features of nanometer-thick films, atomically thin materials, and cell membranes, significantly affecting their elastic properties. Despite decades of theoretical studies on the mechanics of suspended thermalized sheets, controversy still exists over the impact of these ripples, with conflicting predictions about whether elasticity is scale-dependent or scale-independent. Experimental progress has been hindered so far by the inability to have a platform capable of fully isolating and characterizing the effects of ripples. This knowledge gap limits the fundamental understanding of thin materials and their practical applications. Here, we show that thermal-like static ripples shape thin films into a class of metamaterials with scale-dependent, customizable elasticity. Utilizing a scalable semiconductor manufacturing process, we engineered nanometer-thick films with precisely controlled frozen random ripples, resembling snapshots of thermally fluctuating membranes. Resonant frequency measurements of rippled cantilevers reveal that random ripples effectively renormalize and enhance the average bending rigidity and sample-to-sample variations in a scale-dependent manner, consistent with recent theoretical estimations. The predictive power of the theoretical model, combined with the scalability of the fabrication process, was further exploited to create kirigami architectures with tailored bending rigidity and mechanical metamaterials with delayed buckling instability.

Applied Physical Sciences↗
DOE OSTI2024

The influence of electrode crack dimensions on the durability of polymer electrolyte membrane fuel cells

Electrode cracks in polymer electrolyte membrane fuel cells (PEMFCs) are correlated with early onset failures. Here, in this work we investigate the influence of cracked gas diffusion electrodes (GDEs) on the durability of the membrane electrode assembly (MEA) using a combined chemical-mechanical accelerated stress test (AST). Electrode crack dimensions were systematically tuned using ink formulations and material selection strategies. A parameter to describe the crack width areal density (Φ CW ) was used to quantify the degree of discontinuity in the electrode surfaces. Open circuit voltage (OCV) transient analyses were used to benchmark and characterize the failure mechanisms in the MEAs as a function of the Φ CW . While smaller electrode-level cracks, on the order of microns, yielded a 28 % decrease in operating lifetime, larger cracks that propagated from a discontinuous, microporous layer (MPL) coating, decreased the operating lifetime by 56 %. This work emphasizes the need for material processing strategies that consider defect tolerances to limit membrane failures in PEMFCs.

08 HYDROGEN↗
DOE OSTI2025

Characterization of Tank 9H Annulus Sample in Support of Residual Material Inventory Determinations

The Savannah River National Laboratory (SRNL) was requested by Savannah River Mission Completion (SRMC) to provide sample preparation and characterization of the Tank 9H annulus sample in support of Residual Material Inventory Determinations. One Tank 9H sample in three vials [HTF-9-25-13, HTF-9-25-14 and HTF-9-25-15], with each vial containing approximately 200 mL of the Tank 9H annulus salt solution, were delivered to the SRNL Shielded Cells for sample preparation and characterizations in February 2025. The density of the “as-received” solution contained in each of the three Tank 9H annulus sample vials were determined followed by a solid-liquid separation on each one using 0.45-micron Nalgene® nylon filter membranes. The resulting filtrates were combined to form the Tank 9H annulus sample with a total volume of about 600 mL. The combined wet solid fractions, about a total of 4.8 grams of salt material, remaining on the filter membranes were air-dried in the Shielded Cells for 72 hours. The total weight of the air-dried solids was 2.1 grams. These air-dried solids were washed with deionized water (DI water) at a phase ratio of 60 mL DI water/gram of solids to recover insoluble solids, if any. No visible or measurable quantity of insoluble solids were recovered after DI water washing of the air-dried solids because the air-dried solids completely dissolved in the DI water. The solid fraction-wash water was not combined with the 600 mL of the filtrate solution, and the resulting solution was not screened or analyzed for radionuclides. Aliquot sample volumes of the undiluted Tank 9H annulus sample were sent to the SRNL analytical services groups for radionuclides, elementals, anions and total mercury analysis by various methods including radiochemical separations/counting methods, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) and special preparations. All sample analyses were performed in triplicate. This report presents the analytical characterization results for the Tank 9H annulus sample. The results are also reported where analytical methods yielded additional analytes, other than those requested by SRMC. In the characterization of the Tank 9H annulus sample, the detection limits for all the analytes, as specified in the Technical Task Request (TTR) and Task Technical and Quality Assurance Plan (TTQAP), were met.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Degradation of Fuel Cell Membrane Electrode Assemblies from Buses Operated More than 25,000 h

This study investigates the performance losses and degradation of proton-exchange-membrane fuel-cell stacks taken from the Alameda Contra Costa Transit District (AC Transit) bus system (Alameda and Contra Costa counties, California, United States) that were operated for over 25,000 h. Here, we focus on the origin of differences in electrochemical performance between beginning-of-life (BOL) and end-of-life states as well as diagnostic data acquired during the lifetime of the buses. In doing so, we employ in- and ex- situ characterization methods such as polarization curves, electrochemical impedance spectroscopy, electron microscopy, and X-ray characterization. Uniform degradation of the catalyst layer including Pt agglomeration/migration and electrode thinning was observed in all of the post-teardown measurements compared to BOL materials resulting from years of field operation. Despite these changes, the measured post-teardown performance suggests a sufficient output for the expected load, which indicate factors other than degradation of the membrane-electrode assemblies (MEAs) are likely responsible for the decommissioning of the stacks. The findings indicate that these MEA materials can enable long lifetime in fuel-cell vehicles, if the MEAs are not subjected to adverse operating conditions. The results also highlight the need for more in-vehicle diagnostics to maximize the lifetime of fuel cell vehicle (FCV) powerplants.

25 ENERGY STORAGE↗
DOE OSTI2026

Translating Fundamental Insights into Ag-Based Bimetallic Electrocatalysts to Anion-Exchange Membrane Fuel Cells

To address challenges of high costs and scalability for fuel cells, it is essential to develop af-fordable and earth-abundant materials that are Pt-group-metal (PGM)-free. Recent advance-ments in PGM-free electrocatalysis for the oxygen reduction reaction (ORR) in alkaline media show that high catalyst loadings are needed to achieve high reaction rates; however, there are associated mass transport limitations. To address this issue, we develop low-loading ionomer-less Ag-bimetallic thin films by alloying with 3d block elements or Sn. We bridge knowledge from fundamental rotating disk electrode (RDE) studies to gas-diffusion cathodes in high-temperature anion-exchange membrane fuel cells (HT-AEMFCs), resulting in high-activity ORR catalysis and peak power densities up to 1.2 W cm-² geo for the Ag-Sn and Ag-Co alloys. Here, experimental post-characterization and theoretical calculations reveal small Co or Sn oxide nano-islands on Ag as likely active sites enhancing ORR activity, ultimately offering these low-loading PGM-free ORR materials as a viable path towards sustainable energy conversion.

Catalysts↗
DOE OSTI2024

Visualizing plasmons and ultrafast kinetic instabilities in laser-driven solids using X-ray scattering

Ultra-intense lasers that ionize atoms and accelerate electrons in solids to near the speed of light can lead to kinetic instabilities that alter the laser absorption and subsequent electron transport, isochoric heating, and ion acceleration. These instabilities can be difficult to characterize, but X-ray scattering at keV photon energies allows for their visualization with femtosecond temporal resolution on the few nanometer mesoscale. Here, we perform such experiment on laser-driven flat silicon membranes that shows the development of structure with a dominant scale of 60 nm in the plane of the laser axis and laser polarization, and 95 nm in the vertical direction with a growth rate faster than 0.1 fs -1 . Combining the XFEL experiments with simulations provides a complete picture of the structural evolution of ultra-fast laser-induced plasma density development, indicating the excitation of plasmons and a filamentation instability. Particle-in-cell simulations confirm that these signals are due to an oblique two-stream filamentation instability. These findings provide new insight into ultra-fast instability and heating processes in solids under extreme conditions at the nanometer level with possible implications for laser particle acceleration, inertial confinement fusion, and laboratory astrophysics.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2025

Rapid Sensing to Facilitate Purification of Rare Earth Element-Containing Process Streams Produced Through Membrane-Assisted Solvent Extraction

The development of an economically competitive domestic supply of rare earth elements and yttrium (REY) is necessary for our nation’s economic growth and national security. The achievement of a secure domestic supply of REY requires not only the development of effective processes for recovery of REY from naturally occurring materials and/or recycled products, but also the development of downstream processes for the ultimate production of high-REY content solids. An impediment to the development of such processes is the scarcity of analytical methods that provide rapid determination of the process stream compositions. In this work, a membrane-based extraction process was used to selectively recover REYs from a dilute solution in the presence of much higher concentrations of Ca and Al. In tandem, the use of a portable spectrometer equipped with an immobilized zinc adeninate benzene tricarboxylate metal-organic framework sensing material makes possible the rapid detection of the presence of ppm concentrations of Tb and Eu in both weakly acidic and strongly acidic process streams within minutes. A solvent extraction processing time of 15-60 min maximized REY selectivity over gangue ions while achieving up to 80% REY and minimal gangue ion recovery. Taken together, these experiments highlight not only an innovative method for REY purification but also the importance of inexpensive, portable characterization methods for near real-time analysis of REY content.

Membrane-assisted solvent extraction↗
DOE OSTI2025

Vitamin E Acetate Causes Softening of Pulmonary Surfactant Membrane Models

The popularity of electronic cigarettes and vaping products has launched the outbreak of a condition affecting the respiratory system of users, known as electronic-cigarette/vaping-associated lung injury (EVALI). The build-up of vitamin E acetate (VEA), a diluent of some illicit vaping oils, in the bronchoalveolar lavage of patients with EVALI provided circumstantial evidence as a target for investigation. In this work, we provide a fundamental characterization of the interaction of VEA with lung cells and pulmonary surfactant (PS) models to explore the mechanisms by which vaping-related lung injuries may be present. We first confirm the localization and uptake of VEA in pulmonary epithelial cells. Further, as PS is vitally responsible for the biophysical functions of the lungs, we explore the effect of added VEA on three increasingly complex models of PS: dipalmitoylphosphatidylcholine (DPPC), a lipid-only synthetic PS, and the biologically derived extract Curosurf. Using high-resolution techniques of small-angle X-ray scattering, small-angle neutron scattering, neutron spin–echo spectroscopy, and neutron reflectometry, we compare the molecular-scale behaviors of these membranes to the bulk viscoelastic properties of surfactant monolayer films as studied by Langmuir monolayer techniques. While VEA does not obviously alter the structure or organization of PS membranes, a consistent softening of membrane systems—regardless of compositional complexity—provides a biophysical explanation for the respiratory distress associated with EVALI and yields a new perspective on the behavior of the PS system.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Untargeted Spatial Metabolomics and Spatial Proteomics on the Same Tissue Section

An increasing number of spatial multiomic workflows have been recently developed. Some of these approaches have leveraged initial mass spectrometry imaging (MSI)-based spatial metabolomics to inform region of interest (ROI) selection for downstream spatial proteomics. However, these workflows have been limited by varied substrate requirements between modalities or have required analyzing serial sections (i.e., one section per modality). To mitigate these issues, we present a novel multiomic workflow that uses desorption electrospray ionization (DESI)-MSI to identify representative spatial metabolite patterns on-tissue prior to spatial proteomic analyses on the same tissue section. Further, this workflow is demonstrated here with a model mammalian tissue (coronal rat brain section) mounted on a polyethylene naphthalate-membrane slide. Initial DESI-MSI resulted in 160 annotations (SwissLipids) within to the METASPACE platform (≤20% false discovery rate). A segmentation map from the annotated ion images informed downstream ROI selection for spatial proteomics characterization from the same sample. The unspecific substrate requirements and minimal sample disruption inherent to DESI-MSI allowed for an optimized, downstream spatial proteomics assay, resulting in 3888 ± 240 to 4717 ± 48 proteins being confidently directed per ROI (200 µm x 200 µm). Finally, we demonstrate the integration of multiomic information, where we found ceramide localization to be correlated with SMPD3 abundance (ceramide synthesis protein), and we also utilized protein abundance to resolve metabolite isomeric ambiguity. Overall, the integration of DESI-MSI into the multiomic workflow allows for complementary spatial and molecular-level information to be achieved from optimized implementations of each MS assay inherent to the workflow itself.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Infection and Genomic Properties of Single- and Double-Stranded DNA Cellulophaga Phages

Bacterial viruses (phages) are abundant and ecologically impactful, but laboratory-based experimental model systems vastly under-represent known phage diversity, particularly for ssDNA phages. Here, we characterize the genomes and infection properties of two unrelated marine flavophages—ssDNA generalist phage phi18:4 (6.5 Kbp) and dsDNA specialist phage phi18:1 (39.2 Kbp)—when infecting the same Cellulophaga baltica strain #18 (Cba18), of the class Flavobacteriia. Phage phi18:4 belongs to a new family of ssDNA phages, has an internal lipid membrane, and its genome encodes primarily structural proteins, as well as a DNA replication protein common to ssDNA phages and a unique lysis protein. Phage phi18:1 is a siphovirus that encodes several virulence genes, despite not having a known temperate lifestyle, a CAZy enzyme likely for regulatory purposes, and four DNA methyltransferases dispersed throughout the genome that suggest both host modulation and phage DNA protection against host restriction. Physiologically, ssDNA phage phi18:4 has a shorter latent period and smaller burst size than dsDNA phage phi18:1, and both phages efficiently infect this host. These results help augment the diversity of characterized environmental phage–host model systems by studying infections of genomically diverse phages (ssDNA vs. dsDNA) on the same host.

Howard-Varona, Cristina (ORCID:0000000241495818)↗
DOE OSTI2025

Conformational free energy landscape of a glutamate transporter and microscopic details of its transport mechanism

Removing glutamate from the synaptic cleft is vital for proper function of the brain. Excitatory amino acid transporters mediate this process by uptaking the neurotransmitter from the synaptic cleft back to the cell after its release. The archaeal homolog, Glt Ph , an aspartate transporter fromPyrococcus horikoshii, presents the best structurally characterized model for this family of transporters. In order to transport, Glt Ph undergoes elevator-like conformational changes between inward-facing (IF) and outward-facing (OF) states. Here, we characterize, at an atomic level, the OF⇌IF transition of Glt Ph in differentapo/bound states using a combination of ensemble-based enhanced sampling techniques, employing more than two thousand of coupled simulation replicas of membrane-embedded Glt Ph . The resulting free-energy profiles portray the transition ofapo/bound states as a complex four-stage process, while sodium binding alone locks the structure in one of its states. Along the transition, the transport domain (TD) disengages from the scaffold domain (SD), allowing it to move as a piston sliding vertically with respect to the membrane during the elevator-like motion of TD. Lipid interactions with residues comprising the SD–TD interface directly influence the large-scale conformational changes and, consequently, the energetics of transport. Structural intermediates formed during the transition leak water molecules and may correlate to the uncoupled Cl − ion conductance observed experimentally in both prokaryotic and mammalian glutamate transporters. Mechanistic insights obtained from our study provide a structural framework for better development of therapeutic for neurological disorders.

Science & Technology - Other Topics↗
DOE OSTI2025

Structure–property relationships of reduced graphene oxide membranes intercalated with polycyclic aromatics

Graphene oxide (GO) membranes intercalated with various organic moieties have shown excellent potential for a range of water processing applications. However, microstructure–functional property relationships in these structurally disordered membranes are not well understood. We demonstrate a practical methodology for developing such relationships for GO membranes intercalated with molecular species, with polycyclic aromatic toluidine blue O (TBO) as an example functional intercalant. We use solid-state UV–vis absorbance and fluorescence measurements to quantitatively track the arrangements of TBO in a series of TBO-loaded reduced GO (rGO) membranes. This study reveals the evolution of diverse arrangements including TBO monomers, lateral and stacked dimers, and other aggregates, as a function of overall TBO loading. These microstructures are then correlated to changes in overall properties such as interlayer d-spacings, permeate fluxes, and solute rejections. The characterization of these different intercalant microstructures explains non-intuitive flux and rejection trends, which can circumvent flux and solute rejection trade-offs.

02 PETROLEUM↗
DOE OSTI2026

Strain and Defect-Tailored Magnetotransport in NiCo 2 O 4 Thin Films and Freestanding Membranes

Magnetic spinel NiCo 2 O 4 is promising for developing spintronic applications due to its high magnetic Curie temperature, high spin polarization, fast spin dynamics, and strain-tunable magnetic anisotropy, while its electronic and magnetic properties depend sensitively on epitaxial strain and disorder. Here, in this study, we use epitaxial NiCo 2 O 4 thin films and freestanding NiCo 2 O 4 membranes as model systems to reveal the complex interplay of strain and defects in determining the metallicity and magnetotransport properties of the ferrimagnetic spinel. NiCo 2 O 4 on perovskite substrates and NiCo 2 O 4 membranes exhibit insulating behaviors and spin canting, in sharp contrast to the metallic NiCo 2 O 4 films on spinel substrates that possess strong perpendicular magnetic anisotropy. Anisotropic magnetoresistance studies provide critical information about disorder-induced spin scattering and strain-induced tetragonal magnetocrystalline anisotropy, which is corroborated by comprehensive electron microscopy characterizations. Our study presents a promising venue for designing flexible magnetic memory, sensor, and spintronic applications.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Mesoporous Thin Film Architectures: Addressing Material Demands through Molecular Self-Assembly

Mesoporous thin films spark interest across a wide range of disciplines due to their tunable nanostructures, large internal surface areas, and strong compatibility with planar optical, electronic, and microfluidic devices. While attention in the porous materials community has shifted toward macroporous or disordered nanoporous systems, a resurgence in mesoporous thin film research is underway, driven by new molecular self-assembly methods, advanced materials chemistry, and improved characterization techniques. The integration of high-χN block copolymer design, kinetically persistent micelle templating, and postdeposition processing protocols now allows control over structural parameters such as pore size, wall thickness, porosity, and connectivity. These advances have overcome many of the thermodynamic and processing constraints that previously limited widespread adoption. Rather than serving only as high-surface-area supports, mesoporous thin films are engineered as active interfaces where responsive chemistries and nanoscale confinement act in tandem. Embedding switchable ligands, thermoresponsive polymers, redox mediators, or ion-selective groups directly within the pore walls enables real-time control over transport, optical, and electrochemical properties. These capabilities open up new directions in adaptive coatings, gated membranes, and fast-response biosensors. To further expand their functional scope, mesoporous films are integrated into hierarchical and multicomponent architectures. Techniques such as triblock terpolymer templating, crack-directed assembly, and nanoimprint lithography allow for control over spatial organization on the micron and submicron scale and pore system orientation. This enables programmable anisotropy, enhanced molecular diffusion, and wavelength-selective photonic behavior, essential for next-generation sensing, catalysis, and energy applications. Such structural and functional complexity requires equally sophisticated characterization. Multimodal and in situ techniques can track material dynamics under operational conditions. Recent progress includes extended-range ellipsometric porosimetry (EP) for hierarchical architectures, vacuum EP for interface energetics, time-resolved EP for diffusion kinetics, and correlative AFM-SAXS mapping. The introduction of advanced neutron-based spectroscopies, particularly quasielastic neutron scattering (QENS), promises to provide real-time access to ion transport dynamics and segmental motion under nanoscale confinement, offering a path toward deeper mechanistic understanding of structure-performance correlations in mesoporous systems. This Account reflects the technical advances made and the interdisciplinary collaborations that have shaped our collective vision. The particular dimensions of mesopores enable us to subtly tune interactions at the molecular, interfacial, and mesoscopic levels that permit us to harness nanoconfinement. What emerges is a versatile, modular platform capable of chemical gating, energy transduction, and sensing with a level of tunability unmatched by other porous materials. We highlight critical challenges including the need for more robust large-area processing, a deeper understanding of dynamic behavior under cycling, and better integration with device-level architectures. Our strategies support the transition of mesoporous thin films into active high-performance components in next-generation energy, environmental, and biomedical systems.

oxides↗
DOE OSTI2025

Robust Oxygen‐Vacancy‐Engineered Co(OH) 2 /Cu Heterostructures Boost Nitrate Electroreduction to Ammonia beyond 2 A cm −2

Electrocatalytic nitrate reduction reaction (NO 3 RR) presents a sustainable paradigm for green NH 3 synthesis and NO 3 − wastewater valorization. However, overcoming sluggish NO 3 RR kinetics under industrial-current operation persists as a critical challenge. Herein, robust oxygen vacancy-enriched heterostructures (O v -Co(OH) 2 /Cu) are engineered through in situ electrochemical reconstruction. By coupling Cu-mediated NO 3 − -to-NO 2 − conversion with O v -Co(OH) 2 -accelerated NO 2 − -to-NH 3 transformation, this heterostructured system delivers an unprecedented NH 3 yield rate of 167.8 mg h −1 cm −2 and 97.7% Faradaic efficiency at >2 A cm −2 , while maintaining exceptional current tolerance over 25 h. Operando spectroscopic characterizations and theoretical calculations reveal that the introduction of O v in Co(OH) 2 synergistically accelerates water dissociation to ensure continuous hydrogen supply and optimizes *NOOH adsorption, reducing the energy barrier for the rate-limiting step (*NO 2 to *NOOH). To demonstrate practical viability, a membrane-electrode-assembly electrolyzer integrating NO 3 RR with glycerol oxidation reaction achieves highly effective co-production of NH 3 and formate alongside wastewater treatment. In conclusion, this work offers new insights into the rational design of electrocatalysts through in situ reconstruction-induced vacancy engineering for scalable and practical NO 3 RR applications.

ammonia synthesis↗