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DOE OSTI2024

Surface-mediated spontaneous emulsification of the acylated peptide, semaglutide

Acylated peptides composed of glucagon-like peptide-1 receptor agonists modified with a fatty acid side chain are an important class of therapeutics for type 2 diabetes and obesity but are susceptible to an unusual physical instability in the presence of hydrophobic surfaces, i.e., spontaneous emulsification, also known as ouzo formation in practice. In this work, light scattering, small-angle X-ray scattering, and circular dichroism measurements are used to characterize the physical properties of the semaglutide colloidal phase, including size distribution, shape, secondary structure, internal structure, and internal composition, as a function of solution physico-chemical conditions. The existence and size of the colloids formed are successfully predicted by a classical Rayleigh model, which identifies the parameters controlling their size and formation. Colloid formation is found to be catalyzed by hydrophobic surfaces, and formation rates are modeled as an autocatalytic reaction, enabling the formation of a master curve for various surfaces that elucidates the mechanism. Surfaces differ due to differences in surface wettability, which can be correlated with Hansen solubility parameters. This work provides insights into this unusual colloidal phenomenon and guides the peptide synthesis process and drug product formulation in the pharmaceutical industry.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2026

Average hydrodynamic radius analysis reveals critical solvation thresholds in high-concentration lithium electrolytes

Understanding the solvation structures of lithium salts in carbonate- and ether-based electrolytes is central to explaining the exceptional stability of high-concentration electrolytes (HCEs) and localized high-concentration electrolytes (LHCEs). Conventional techniques such as vibrational spectroscopy and one-dimensional NMR provide only limited information, typically restricted to coordination ratios and ion-pair distributions, without revealing the actual size and mass of solution complexes. Here, in this study, we introduce an average hydrodynamic radius (AHR) analysis based on internally referenced DOSY NMR, which enables direct estimation of the average volume and molecular weight of lithium–solvent complexes in solution. Using LiFSI–EMC and LiFSI–EMC–TTE electrolytes, we demonstrate that the onset of effective lithium metal stabilization and aluminum corrosion suppression coincides with the formation of very large complexes, whose average volume exceeds 300 times that of free EMC molecules. This finding supports a new “blocking mechanism,” wherein bulky solvated complexes impede direct solvent access to reactive surfaces. The AHR analysis thus not only clarifies the fundamental origin of HCE and LHCE effectiveness, but also provides a broadly applicable experimental framework for probing complex solvation structures and guiding rational electrolyte design.

Concentrated electrolytes↗

DOE OSTI2015

Effects of Dopant Metal Variation and Material Synthesis Method on the Material Properties of Mixed Metal Ferrites in Yttria Stabilized Zirconia for Solar Thermochemical Fuel Production

Mixed metal ferrites have shown much promise in two-step solar-thermochemical fuel production. Previous work has typically focused on evaluating a particular metal ferrite produced by a particular synthesis process, which makes comparisons between studies performed by independent researchers difficult. A comparative study was undertaken to explore the effects different synthesis methods have on the performance of a particular material during redox cycling using thermogravimetry. This study revealed that materials made via wet chemistry methods and extended periods of high temperature calcination yield better redox performance. Differences in redox performance between materials made via wet chemistry methods were minimal and these demonstrated much better performance than those synthesized via the solid state method. Subsequently, various metal ferrite samples (NiFe 2 O 4 , MgFe 2 O 4 , CoFe 2 O 4 , and MnFe 2 O 4 ) in yttria stabilized zirconia (8YSZ) were synthesized via coprecipitation and tested to determine the most promising metal ferrite combination. It was determined that 10 wt.% CoFe 2 O 4 in 8YSZ produced the highest and most consistent yields of O 2 and CO. By testing the effects of synthesis methods and dopants in a consistent fashion, those aspects of ferrite preparation which are most significant can be revealed. More importantly, these insights can guide future efforts in developing the next generation of thermochemical fuel production materials.

Leonard, Jeffrey↗

NASA NTRS1987

Shuttle bay telerobotics demonstration

A demonstration of NASA's robotics capabilities should be a balanced agenda of servicing and assembly tasks combined with selected key technical experiments. The servicing tasks include refueling and module replacement. Refueling involves the mating of special fluid connectors while module replacement requires an array of robotic technologies such as special tools, the arm of a logistics tool, and the precision mating of orbital replacement units to guides. The assembly task involves the construction of a space station node and truss structure. The technological experiments will focus on a few important issues: the precision manipulation of the arms by a teleoperator, the additional use of several mono camera views in conjunction with the stereo system, the use of a general purpose end effector versus a caddy of tools, and the dynamics involved with using a robot with a stabilizer.

Chun, W.↗

NASA NTRS2021

System Analysis and Generative Design for Icenode, a Buoyant Vehicle for Measuring Melt Rate Under Ice Shelves

Antarctic ice shelves buttress the Antarctic Ice Sheet from sliding into the ocean, and their collapse could trigger a meter or more of global sea level rise by the end of the century. Current state-of-the-art predictions for ice shelf behavior in a warming climate have large uncertainty, significantly hindered by a lack of in situ melt rate observations under ice shelves, especially near grounding zones. IceNode is a novel robotic vehicle under development at the NASA Jet Propulsion Laboratory to acquire such measurements, but presents a complex design problem owing to the large design space and conflicting performance requirements. Evaluating a preliminary design requires several types of tedious analysis which prevents rapid iteration and exploration of the design space. We present the implementation of a custom system analysis framework which was used to automate analysis such as resource budgeting, mission simulation, mass and buoyancy balancing, and static landing stability analysis of a given design configuration. Using this framework, we selected parameters which had the largest effects on design success and conducted a generative design study in which we programmatically varied a handful of parameters to generate 1540 different design candidates and test them across 160 different environmental scenarios. The custom built system analysis tool enabled rapid development of critical analysis and automated exploration of a large design space to guide preliminary design of the IceNode vehicle.

Gebara, Christine↗

NASA NTRS1924

Static stability of seaplane floats and hulls

Values of lateral and longitudinal metacentric heights for various seaplanes were calculated by means of approximate formulae derived here. The data are given in tabular form. Upon plotting these metacentric heights against the corresponding gross weights, it appears that the metacentric height is approximately a straight line function of the gross weight. For the lateral metacentric height GM = 13 + .002 W and for longitudinal metacentric height GM = 15 + .002 W, GM is in feet and the gross weight (W) is in pounds. Although only approximate, it is thought that the values indicated here are a reliable guide to current practice. It is recommended that the longitudinal and lateral metacentric heights be made equal and of the value given by GM = 15 = .002 W. The proper length or spacing required to satisfy the indicated value may then be obtained from substitution in the approximate formulae for metacentric height.

Diehl, W S↗

DOE OSTI2020

Precipitation Trade Wind Cumuli within EUREC 4 A Field Campaign Report

The campaign Trades Cumuli Precipitation Initiation and Characterization (TCPIC) within the overarching Elucidating the Role of Clouds-Circulation Coupling in Climate EUREC 4 A campaign took place from 17 January 2020 to 20 February 2020, a total of 35 days. The campaign complemented the more extensive EUREC 4 A campaign focusing on cumulus clouds' role in the Earth's climate. TCPIC concentrated on understanding what triggers the onset and development of precipitation in trade wind cumulus clouds. The campaign requested the deployment of the U.S. Department of Energy Atmospheric Radiation Measurement (ARM) Mobile Facility (AMF) roll, pitch, and heave (RPH) stabilization platform to stabilize two radars on the Maria S. Merian research vessel (RV). The advanced remote-sensing techniques from stabilized radars characterized the entire precipitation life cycle, from the formation of larger cloud drops to precipitation evaporating on its way to the surface. Retrievals of evaporation rates, to track how rain affects the trade wind boundary layer, will be based on the zenith-pointing Doppler observations collected from the stabilized micro rain radar (MRR). Figure 1 shows the instrumentation's deployment on the RV: we installed the AMF RPH stabilization platform and the radars on the uppermost deck (peil deck) of the ship. For installing the devices, we coordinated a test phase of the equipment on the Maria S. Merian RV from 25 to 29 October 2019 in Emden harbor, Germany. In this testing phase, we set up all the connections, tested how to mount the W-band and the micro rain radars firmly on the table, and experimented with guided movements of the table to test the resistance of the whole system. Figure 1 shows the final tests conducted in Emden with the stable platform and the radars mounted.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2026

Advances in genetic tools for metabolic engineering of non-conventional yeasts

Non-conventional yeasts are emerging as powerful alternatives to Saccharomyces cerevisiae for metabolic engineering, owing to their innate stress tolerance, broad substrate utilization, and distinctive metabolic capabilities. These attributes position them as promising chassis for producing biofuels, pharmaceuticals, and specialty chemicals. This review synthesizes recent advances in genetic toolkits for four such species—Pichia kudriavzevii (Issatchenkia orientalis), Starmerella bombicola, Debaryomyces hansenii, and Pachysolen tannophilus—highlighting progress across plasmid architectures (episomal and integrative), identification of autonomously replicating sequences and centromeric elements, and the development of safe-harbor genomic loci. We summarize promoter and terminator libraries enabling tunable expression, the expansion of auxotrophic and antifungal selection markers with recycling strategies, and the rapid adaptation of CRISPR-based systems (Cas9 and Cas12a) with optimized guide RNA expression, multiplex editing, and approaches that enhance homologous recombination (e.g., KU70/80 disruption). We also review landing-pad platforms for modular, repeated integrations and transposon-based tools (e.g., piggyBac) that facilitate multigene pathway assembly. Collectively, these innovations are accelerating design-build-test-learn cycles and enabling precise, scalable engineering of non-conventional yeasts. Remaining challenges—including limited species-specific episomal systems, variable transformation efficiencies, genome-stability concerns, and alternative codon usage—define clear priorities for future toolkit development. Together, these advances and open needs chart a path toward robust, sustainable biomanufacturing using diverse non-conventional yeast chassis.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS1999

Endoscopic surgery and telemedicine in microgravity: developing contingency procedures for exploratory class spaceflight

OBJECTIVES: The risk of a urinary calculus during an extended duration mission into the reduced gravity environment of space is significant. For medical operations to develop a comprehensive strategy for the spaceflight stone risk, both preventive countermeasures and contingency management (CM) plans must be included. METHODS: A feasibility study was conducted to demonstrate the potential CM technique of endoscopic ureteral stenting with ultrasound guidance for the possible in-flight urinary calculus contingency. The procedure employed the International Space Station/Human Research Facility ultrasound unit for guide wire and stent localization, a flexible cystoscope for visual guidance, and banded, biocompatible soft ureteral stents to successfully stent porcine ureters bilaterally in zero gravity (0g). RESULTS: The study demonstrated that downlinked endoscopic surgical and ultrasound images obtained in 0g are comparable in quality to 1g images, and therefore are useful for diagnostic clinical utility via telemedicine transmission. CONCLUSIONS: In order to be successful, surgical procedures in 0g require excellent positional stability of the operating surgeon, assistant, and patient, relative to one another. The technological development of medical procedures for long-duration spaceflight contingencies may lead to improved terrestrial patient care methodology and subsequently reduced morbidity.

Parabolic Flight↗

DOE OSTI2019

Comparing Ocean Surface Boundary Vertical Mixing Schemes Including Langmuir Turbulence

Six recent Langmuir turbulence parameterization schemes and five traditional schemes are implemented in a common single-column modeling framework and consistently compared. These schemes are tested in scenarios versus matched large eddy simulations, across the globe with realistic forcing (JRA55-do,WAVEWATCH-III simulated waves) and initial conditions (Argo), and under realistic conditions as observed at ocean moorings. Traditional non-Langmuir schemes systematically underpredict large eddy simulation vertical mixing under weak convective forcing, while Langmuir schemes vary in accuracy. Under global, realistic forcing Langmuir schemes produce 6% (–1% to 14% for 90% confidence) or 5.2 m (–0.2 m to 17.4 m for 90% confidence) deeper monthly mean mixed layer depths than their non-Langmuir counterparts, with the greatest differences in extratropical regions, especially the Southern Ocean in austral summer. Discrepancies among Langmuir schemes are large (15% in mixed layer depth standard deviation over the mean): largest under wave-driven turbulence with stabilizing buoyancy forcing, next largest under strongly wave-driven conditions with weak buoyancy forcing, and agreeing during strong convective forcing. Non-Langmuir schemes disagree with each other to a lesser extent, with a similar ordering. Langmuir discrepancies obscure a cross-scheme estimate of the Langmuir effect magnitude under realistic forcing, highlighting limited understanding and numerical deficiencies. Maps of the regions and seasons where the greatest discrepancies occur are provided to guide further studies and observations.

58 GEOSCIENCES↗

DOE OSTI2026

Chemical factors controlling the behaviour of oxide cathodes in batteries

Oxide cathodes enable high-energy lithium-ion and sodium-ion batteries, with their performances fundamentally governed by three interrelated chemical factors: electronic configuration, chemical bonding, and chemical reactivity. Here, we illustrate how these factors dictate the redox energy, structural stability, ionic and electronic transport, and interfacial behavior in both layered oxide and polyanion oxide cathodes. We discuss how crystal-field effects and octahedral-site stabilization energies influence cation migration, and how inductive effects tune bond covalency and operating voltages. We also explain how chemical bonding governs thermal stability, gas evolution, and first-cycle capacity loss, and how alignment of transition-metal redox band with the oxygen 2p band determines electrolyte reactivity. Comparison between lithium and sodium layered oxides further reveals how differences in Li-O and Na-O bond ionicity affect chemical reactivity. Finally, we outline strategies including compositional tuning, surface doping, and electrolyte optimization, and emphasize how high-throughput, data-driven approaches in guiding the design of next-generation oxide cathodes.

25 ENERGY STORAGE↗

NASA NTRSDate not supplied

Anisotropic Goal-Based Mesh Adaptation Metric Clarification and Development

Adaptive unstructured mesh techniques have a limited, but growing impact on production analysis workflows to control discretization error for reliable simulation results. Multiple independent implementations of flow solvers, anisotropic metric construction methods, and anisotropic mesh adaptation mechanics have matured. Goal-based metrics target estimated error in output functions, such as lift and drag, through the guidance of an adjoint solution. A unification of goal-based anisotropic metrics is presented for steady viscous flows, which is an active area of research. These goal-based metrics drive robust and efficient anisotropic mesh adaptation for the calculation of output functions. The super-convergent functional output error behavior of stabilized finite-element methods is exploited without a formal proof, and evidence of super-convergence is shown in numerical experiments. Mesh adapted drag and lift outputs for two simple bodies in compressible viscous flow show convergence of error to less than a single drag count. Asymptotic behavior established for relatively coarse meshes shows the efficiency of this goal-based metric when compared to solution interpolation error control and expert-guided meshing. Anisotropic mesh adaptation techniques are applied to a transport aircraft in a high-lift configuration where variation between approaches decreases with mesh refinement, but asymptotic behavior is not observed with available resources.

goal-based↗

DOE OSTI2020

Nanocomposite Ionogel Electrolytes for Solid‐State Rechargeable Batteries

Abstract Ionogels composed of ionic liquids and gelling solid matrices offer several advantages as solid‐state electrolytes for rechargeable batteries, including safety under diverse operating conditions, favorable electrochemical and thermal properties, and wide processing compatibility. Among gelling solid matrices, nanoscale materials have shown particular promise due to their ability to concurrently enhance ionogel mechanical properties, thermal stability, ionic conductivity, and electrochemical stability. These beneficial attributes suggest that ionogel electrolytes are not only of interest for incumbent lithium‐ion batteries but also for next‐generation rechargeable battery technologies. Herein, recent advances in nanocomposite ionogel electrolytes are discussed to highlight their advantages as solid‐state electrolytes for rechargeable batteries. By exploring a range of different nanoscale gelling solid matrices, relationships between nanoscale material structure and ionogel properties are developed. Furthermore, key research challenges are delineated to help guide and accelerate the incorporation of nanocomposite ionogel electrolytes in high‐performance solid‐state rechargeable batteries.

Hyun, Woo Jin↗

DOE OSTI2015

Laboratory Experiments and Instrument Intercomparison Studies of Carbonaceous Aerosol Particles

Aerosols containing black carbon (and some specific types of organic particulate matter) directly absorb incoming light, heating the atmosphere. In addition, all aerosol particles backscatter solar light, leading to a net-cooling effect. Indirect effects involve hydrophilic aerosols, which serve as cloud condensation nuclei (CCN) that affect cloud cover and cloud stability, impacting both atmospheric radiation balance and precipitation patterns. At night, all clouds produce local warming, but overall clouds exert a net-cooling effect on the Earth. The effect of aerosol radiative forcing on climate may be as large as that of the greenhouse gases, but predominantly opposite in sign and much more uncertain. The uncertainties in the representation of aerosol interactions in climate models makes it problematic to use model projections to guide energy policy. The objective of our program is to reduce the uncertainties in the aerosol radiative forcing in the two areas highlighted in the ASR Science and Program Plan. That is, (1) addressing the direct effect by correlating particle chemistry and morphology with particle optical properties (i.e. absorption, scattering, extinction), and (2) addressing the indirect effect by correlating particle hygroscopicity and CCN activity with particle size, chemistry, and morphology. In this connection we are systematically studying particle formation, oxidation, and the effects of particle coating. The work is specifically focused on carbonaceous particles where the uncertainties in the climate relevant properties are the highest. The ongoing work consists of laboratory experiments and related instrument inter-comparison studies both coordinated with field and modeling studies, with the aim of providing reliable data to represent aerosol processes in climate models. The work is performed in the aerosol laboratory at Boston College. At the center of our laboratory setup are two main sources for the production of aerosol particles: (a) two well-characterized source of soot particles and (b) a flow reactor for controlled OH and/or O3 oxidation of relevant gas phase species to produce well-characterized SOA particles. After formation, the aerosol particles are subjected to physical and chemical processes that simulate aerosol growth and aging. A suite of instruments in our laboratory is used to characterize the physical and chemical properties of aerosol particles before and after processing. The Time of Flight Aerosol Mass Spectrometer (ToF-AMS) together with a Scanning Mobility Particle Sizer (SMPS) measures particle mass, volume, density, composition (including black carbon content), dynamic shape factor, and fractal dimension. The–ToF-AMS was developed at ARI with Boston College participation. About 120 AMS instruments are now in service (including 5 built for DOE laboratories) performing field and laboratory studies world-wide. Other major instruments include a thermal denuder, two Differential Mobility Analyzers (DMA), a Cloud Condensation Nuclei Counter (CCN), a Thermal desorption Aerosol GC/MS (TAG) and the new Soot Particle Aerosol Mass Spectrometer (SP-AMS). Optical instrumentation required for the studies have been brought to our laboratory as part of ongoing and planned collaborative projects with colleagues from DOE, NOAA and university laboratories. Optical instruments that will be utilized include a Photoacoustic Spectrometer (PAS), a Cavity Ring Down Aerosol Extinction Spectrometer (CRD-AES), a Photo Thermal Interferometer (PTI), a new 7-wavelength Aethalometer and a Cavity Attenuated Phase Shift Extinction Monitor (CAPS). These instruments are providing aerosol absorption, extinction and scattering coefficients at a range of atmospherically relevant wavelengths. During the past two years our work has continued along the lines of our original proposal. We report on 12 completed and/or continuing projects conducted during the period 08/14 to 0814/2015. These projects are described in 17 manuscripts published in refereed journals.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2016

Band diagram and rate analysis of thin film spinel LiMn 2 O 4 formed by electrochemical conversion of ALD-grown MnO

Nanoscale spinel lithium manganese oxide is of interest as a high-rate cathode material for advanced battery technologies among other electrochemical applications. In this work, the synthesis of ultrathin films of spinel lithium manganese oxide (LiMn 2 O 4 ) between 20 and 200 nm in thickness by room-temperature electrochemical conversion of MnO grown by atomic layer deposition (ALD) is demonstrated. The charge storage properties of LiMn 2 O 4 thin films in electrolytes containing Li + , Na + , K + , and Mg 2+ are investigated. A unified electrochemical band-diagram (UEB) analysis of LiMn 2 O 4 informed by screened hybrid density functional theory calculations is also employed to expand on existing understanding of the underpinnings of charge storage and stability in LiMn 2 O 4 . It is shown that the incorporation of Li + or other cations into the host manganese dioxide spinel structure (λ-MnO 2 ) stabilizes electronic states from the conduction band which align with the known redox potentials of LiMn 2 O 4 . Furthermore, the cyclic voltammetry experiments demonstrate that up to 30% of the capacity of LiMn 2 O 4 arises from bulk electronic charge-switching which does not require compensating cation mass transport. As a result, the hybrid ALD-electrochemical synthesis, UEB analysis, and unique charge storage mechanism described here provide a fundamental framework to guide the development of future nanoscale electrode materials for ion-incorporation charge storage.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Catalytic hydrogenation of HMF to BHMF over copper catalysts

2,5-Bis(hydroxymethyl)furan (BHMF) is a bio-derived building block for polyester production, obtained via the hydrogenation of 5-hydroxymethylfurfural (HMF). First-principles thermodynamic equilibrium calculations indicate that this reaction is not thermodynamically limited under relevant conditions (e.g., 100 °C and high H 2 partial pressure). In this work, crude HMF was employed as the feedstock for BHMF synthesis. Initially, acidic impurities and humins were removed from unrefined HMF through filtration using a packed bed of γ-alumina. A comprehensive study of the filtration process is presented, including filtration kinetics, breakthrough curve analysis, and mathematical modeling. The purified HMF was subsequently hydrogenated over a 10 wt% CuZrO 2 catalyst, using ethanol as the reaction solvent. Batch reactions were first performed for collection of kinetic data to guide the transition to continuous flow operation. Kinetic data was collected in a fixed bed reactor at varying contact time, time on stream, temperature, and HMF concentration. This data was used to develop a kinetic model for HMF hydrogenation. Maximum BHMF production rates were achieved at 130 °C, accompanied by minor formation of byproducts from BHMF ring-opening reactions. The BHMF selectivity was 100 % at 100 °C although with lower reaction rates. Furthermore, catalyst stability tests revealed a loss of up to 50 % in catalytic activity within the first 24 h, likely due to the adsorption of HMF-derived oligomers that are not easily removed by filtration.

Crude HMF filtration↗

DOE OSTI2026

Rational design of heterogeneous single-site catalysts via surface organometallic chemistry

Single-site heterogeneous catalysts offer an attractive route to unite the molecular precision of homogeneous catalysis with the durability and practical advantages of solids. Surface organometallic chemistry (SOMC) provides a particularly powerful strategy for this purpose by grafting molecular precursors onto tailored surfaces and converting support functionalities into ligand environments for isolated metal centers. As a result, SOMC brings the language and logic of coordination chemistry to heterogeneous catalysis, where the support becomes an integral part of the active site coordination sphere. This Review surveys recent progress in the rational design of SOMC-derived single-site catalysts, with emphasis on synthetic routes, post synthetic transformations, and the deliberate tuning of catalytic behavior through metal-support interactions. Discussions are made on how support identity, hydroxyl topology, acidity, and redox activity shape the geometry, electronic structure, and oxidation state of supported metal sites, as well as how these factors determine activity, selectivity, and stability. We also examine a central limitation of these systems: despite their molecularly informed design, supported single sites often exist as structurally distributed ensembles rather than uniform species, particularly on amorphous supports. This site heterogeneity, along with catalyst dynamics under operating conditions, remains a major barrier to definitive structure-activity relationships. Therefore, emerging approaches that combine advanced characterization, first-principles modeling, ensemble kinetics, and machine learning to resolve active-site structure and guide catalyst development are highlighted. Together, these advances position SOMC as a versatile coordination chemistry framework for the predictive design of heterogeneous catalysts with well-defined molecularly tailored active sites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Methanol tolerance of atomically dispersed single metal site catalysts: mechanistic understanding and high-performance direct methanol fuel cells

Proton-exchange membrane fuel cells (PEMFCs) and direct methanol fuel cells (DMFCs) are promising power sources from portable electronic devices to vehicles. The high-cost issue of these low-temperature fuel cells can be primarily addressed by using platinum-group metal (PGM)-free oxygen reduction reaction (ORR) catalysts, in particular atomically dispersed metal–nitrogen–carbon (M–N–C, M = Fe, Co, Mn). Furthermore, a significant advantage of M–N–C catalysts is their superior methanol tolerance over Pt, which can mitigate the methanol cross-over effect and offer great potential of using a higher concentration of methanol in DMFCs. In this work, we investigated the ORR catalytic properties of M–N–C catalysts in methanol-containing acidic electrolytes via experiments and density functional theory (DFT) calculations. FeN 4 sites demonstrated the highest methanol tolerance ability when compared to metal-free pyridinic N, CoN 4 , and MnN 4 active sites. The methanol adsorption on MN 4 sites is even strengthened when electrode potentials are applied during the ORR. The negative influence of methanol adsorption becomes significant for methanol concentrations higher than 2.0 M. However, the methanol adsorption does not affect the 4e - ORR pathway or chemically destroy the FeN 4 sites. The understanding of the methanol-induced ORR activity loss guides the design of promising M–N–C cathode catalyst in DMFCs. Accordingly, we developed a dual-metal site Fe/Co–N–C catalyst through a combined chemical-doping and adsorption strategy. Instead of generating a possible synergistic effect, the introduced Co atoms in the first doping step act as “scissors” for Zn removal in metal–organic frameworks (MOFs), which is crucial for modifying the porosity of the catalyst and providing more defects for stabilizing the active FeN 4 sites generated in the second adsorption step. The Fe/Co–N–C catalyst significantly improved the ORR catalytic activity and delivered remarkably enhanced peak power densities (i.e., 502 and 135 mW cm -2 ) under H 2 –air and methanol–air conditions, respectively, representing the best performance for both types of fuel cells. Notably, the fundamental understanding of methanol tolerance, along with the encouraging DMFC performance, will open an avenue for the potential application of atomically dispersed M–N–C catalysts in other direct alcohol or ammonia fuel cells.

25 ENERGY STORAGE↗