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DOE OSTI2024

Development and Commercialization of a Nanosegrated Oxygen Evolution Reaction Electrocatalyst (CRADA)

This collaborative project leverages advanced characterization tools, catalyst treatment and electrochemical testing capabilities at LBNL to help commercialize a bimetallic nanosegrated catalysts for oxygen evolution reaction in proton-exchange membrane water electrolyzers. This project also has three industrial partners who are involved in catalyst scale-up synthesis, large electrode fabrication and large electrode electrochemical testing. This project investigates a broad range of topics including electrocatalysis, ink rheology and electrode fabrication and testing. This knowledge could help bridge the performance and durability gap from laboratory-developed materials (such as electrocatalysts) to applications in commercial devices. The research results also bring fundamental understanding of possible degradation mechanisms that occur under extremely oxidative potentials including material and morphological changes. The project will help accelerate the deployment of proton-exchange membrane water electrolyzers. The public benefits could include creating jobs and increasing public awareness of potential clean technologies for green hydrogen production. Ultimately, the project will help national wide effort of flighting climate change and achieving carbon neutrality by 2050.

30 DIRECT ENERGY CONVERSION↗

DOE OSTI2024

Additive manufacturing of multiscale NiFeMn multi-principal element alloys with tailored composition

Nanostructured multi-principal element alloys (MPEAs) have been explored as next-generation engineering materials due to unique mechanical and functional properties which have significant advantages over traditional dilute alloys. However, the practical applications of nanostructured MPEAs are still limited due to the lack of scalable processing approaches to prepare a large quantity of nanostructured MPEAs, as well as lack of an efficient pathway for high-throughput discovery of better functional nanostructured MPEAs within their vast compositional space. Here we tackle these challenges by presenting an integrated approach by combining direct-ink-writing-based additive manufacturing, solid-state sintering, and chemical dealloying to manufacture hierarchically porous MPEAs. The hierarchical structure is comprised of macro- and micro-scale pores introduced via extrusion printing and polymer decomposition during sintering, as well as nanoscale pores formed via chemical dealloying. The macro- and micro-scale pores allow efficient dealloying of a large mass of material as the diffusion length that the corroding medium must penetrate remains at the scale of the ligaments formed after sintering (∼10 μm), despite the large volume of the 3D-printed samples. In addition, this integrated approach enables versatile control of the alloy composition via precisely tuning the ratio of elemental powders in the starting ink, thus offering a pathway for high-throughput discovery of novel functional MPEAs. As a case study, multiscale macro/micro/nanoporous NiFeMn MPEAs with three different compositions were investigated as catalysts to reduce the overpotential of oxygen evolution reaction (OER), where NiFeMn-based electrocatalysts display composition-dependent performance such that the overpotential measured at a current of 0.5 A g −1 for OER increases in the order of Ni 58 Fe 29 Mn 13 ⩽ Ni 64 Fe 26 Mn 10 < Ni 76 Fe 18 Mn 6 . This introduced manufacturing process offers new opportunities for scalable fabrication and rapid screening of nanostructured multi-component complex alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Oxygen Reduction on Platinum-Nickel and Platinum-Cobalt Alloy Based Catalysts for High Temperature Proton Exchange Membrane Fuel Cells

Catalyst layers, with commercial PtNi/TKK (TECNiE52; platinum 46.5 wt%), PtCo/TKK (TEC36E52; platinum 45.8 wt%) catalysts, and an in-house catalyst PtNi-NC (platinum 38.4 wt%), synthesised using acoustic mixer and a tube furnace, are prepared using three different ionomers: 20 wt% Nafion®, 60 wt% polytetrafluoroethylene (PTFE), and an in-house 5 wt% ionomer (‘Ionomer X’). These inks are bar-coated onto carbon paper gas diffusion layers (GDLs), which are cut into 3 cm × 5 cm pieces. The coated layers are tested for oxygen reduction in a commercial gas diffusion electrode (GDE) test cell, FlexCell® (Gaskatel GmbH, Germany), using 85 wt% phosphoric acid at both room temperature and at 155°C. This study evaluates the polynorbornene (PNB)-based in-house ionomer performance as binder and in-house catalyst oxygen reduction reaction (ORR) activity in comparison to commercial products. The catalyst layers are characterised using X-ray diffraction (XRD) analysis, X-ray photoelectron spectroscopy (XPS), and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM). Among the catalyst layers prepared with PTFE ionomer and tested at 155°C, the in-house catalyst demonstrates the highest ORR activity. Ionomer X proves to be a good candidate to be used as a per- and polyfluoroalkyl-free binder for high-temperature (HT) proton exchange membrane fuel cell (PEMFC) applications.

85 wt% phosphoric acid↗

DOE OSTI2025

PFSA-Ionomer Dispersions to Thin-Films: Interplay Between Sidechain Chemistry and Dispersion Solvent

In fuel-cell catalyst layers (CLs), ionomers exists as nanoscale thin-films binding catalyst particles, wherein ionic and gaseous species transport to catalyst sites. To improve film function, ionomers have been designed based on the prototypical perfluorosulfonic acid (PFSA). Since CLs are fabricated through solution-based processing of inks, understanding how ink/dispersion solvent impacts ionomer interactions and function is important to guide future ionomer design. Herein, PFSA and its chemical derivatives are characterized from dispersion (in solvent) to thin film (cast on support) to investigate the impact of solvent water content on ionomer dispersion (structure, acidity) and resulting film properties. Dispersion characterization reveals that secondary aggregate structure depends on the sidechain chemistry, but all PFSA-based ionomers evolve similarly as dispersion becomes water-rich. The differences in aggregation alter ionomer adsorption and thin film morphology. Further, hydrophilic domain spacing and orientation are affected primarily by sidechain chemistry, and modulated by solvent composition. Thin-film conductivity correlates with hydration and nanodomain alignment, signifying the role of morphology in properties. Overall, this work provides insights into how chemistry can be used to coarse-tune structure–property relationships, while processing solvent is for fine-tuning of dispersion-film interplay for controlling CL-ionomer function, which can be translated to other chemistries and ink formulations.

25 ENERGY STORAGE↗

DOE OSTI2025

Titanium nitride prepared by the urea-glass synthesis gives an active electrocatalyst for the oxygen reduction reaction

Rock-salt-structured titanium nitride (TiN) has emerged as a leading earth-abundant electrocatalyst for the oxygen reduction reaction (ORR). We compare TiN prepared in three ways starting from urea: the urea–glass method, by a direct reaction between urea and titanium(IV) chloride, and through a discrete monomeric complex. In the urea-glass route, a new-found [Ti 4 (µ-O) 6 (OC(NH 2 ) 2 ) 12 ] 4+ oxo-bridged titanium–urea precursor can be synthesized in a single-pot reaction at room temperature starting from titanium(IV) chloride, urea, and ethanol with a urea-to-titanium ratio of 6. Subsequent annealing of the polymeric gel that results at 750 °C in an N 2 atmosphere yields phase-pure, TiN particles on the 100 µm size scale. TiN can be deposited as an ink with PiperlON®anion exchange dispersion onto a glassy carbon rotating disk electrode (RDE), and of the three synthesis methods, the urea-glass method gives the most active ORR catalyst. The onset potential for ORR activity is −131 mV vs. Hg/HgO, and Koutecký–Levich analysis of linear-sweep voltammetry recorded at varying rotation rates supports a two-electron reduction pathway to H 2 O 2 , with a rate constant of 0.0172 cm s −1 . The higher activity is ascribed to a more oxygen-rich surface—boh defect sites and active oxygen species—afforeded by the oxo-bridged precursor, corrorborated by X-ray photoelectron spectroscopy (XPS) analysis.

Xie, Wanrui [University of Michigan, Ann Arbor, MI↗

DOE OSTI2025

3D printing of architected sulfur cathodes with dual-site atomic catalysts for accelerated polysulfide kinetics and Li-ion transport in high areal-loading lithium–sulfur batteries

The practical deployment of lithium–sulfur batteries (LSBs) is hindered by fundamental limitations in conventional slurry-cast cathodes, including poor sulfur utilization, sluggish ion transport, and low areal capacity, particularly in thick electrodes required for high energy density. To address these challenges, we present direct ink writing (DIW) as an additive manufacturing strategy to fabricate advanced current-collector-free, 3D-printed sulfur cathodes (3DP S@CoNi-DSACs/NC) with hierarchically porous architectures that enhance lithium-ion diffusion, promote electrolyte penetration, and reduce interfacial resistance. The synergistic effects of Co/Ni dual-atom sites accelerate redox kinetics and mitigate polysulfide shuttling. As a result, the optimized 3DP cathode with a sulfur loading of 5.4 mg cm −2 demonstrated excellent rate capability, delivering a high reversible capacity of 1041.4 mAh g −1 at 1C with 85.5% capacity retention after 1000 cycles, significantly outperforming its cast counterpart. Remarkably, even at a higher sulfur loading of 8.1 mg cm −2 , the 3DP cathode maintains outstanding performance, achieving a discharge capacity of 1538.4 mAh g −1 and an areal capacity of 12.5 mAh cm −2 at 0.1C. This study not only demonstrates the functional integration of catalytically active materials into 3D printable sulfur cathode architectures but also offers a scalable and transformative platform for building high-performance LSBs beyond conventional electrode manufacturing methods.

3D electrode↗