Advances in Simultaneous Reduction and Nitriding of Iron Oxides using Ammonia by Harnessing Operando Cross-Scale X-Ray Scattering Measurements

Aug 6, 2026, 11:45 AM
30m
Bradfield 101 (Cornell University)

Bradfield 101

Cornell University

306 Tower Road, Ithaca, NY 14853, USA Cornell University College of Agriculture and Life Sciences
Oral presentation Plants and critical minerals Plants and critical minerals

Speaker

Greeshma Gadikota (Columbia University)

Description

Ammonia is the molecular foundation of the global food system, supplying the nitrogen fertilizer that sustains roughly half the world's population — yet its synthesis consumes an estimated 1–2% of global energy. Iron nitrides are earth-abundant materials central to greening this nitrogen economy: candidate catalysts for nitrogen reduction and ammonia synthesis, ammonia decomposition for hydrogen storage, and rare-earth-free magnets. Each function demands phase-selective control over iron nitride formation, requiring a mechanistic understanding of how iron oxides are simultaneously reduced and nitrided.

Departing from multi-step reduction using carbonaceous resources followed by nitriding, we develop a single-step pathway using ammonia as both reducing and nitriding agent — cheaper to transport than hydrogen and uniquely enabling simultaneous reduction and nitriding to tailor metallic versus nitride products in one step. Using Fe₂O₃ as a case study, we apply operando USAXS/SAXS/WAXS to resolve these poorly understood coupled kinetics from sub-nanometer to micrometer scales, tracking phase evolution alongside morphology relevant to scale-up.

Reducing Fe₂O₃ in ammonia at 500–800 °C reveals a temperature-independent pathway but a temperature-dependent product. Reduction proceeds Fe₂O₃ → Fe₃O₄ → FeO; FeO is then reduced and nitrided to Fe₄N, which decomposes to Fe. Temperature tunes the reduction–nitriding balance: incomplete reduction with mixed Fe/Fe₄N/Fe₃N at 500 °C, single-phase Fe₄N at 600 °C, a Fe/Fe₄N mixture at 700 °C, and pure Fe at 800 °C. USAXS shows agglomeration only at 600–800 °C, with the smoothest surfaces for single-phase products.

This work shows the iron product can be tailored by composition and morphology, establishing operando cross-scale scattering for scale-up of ammonia-based reduction–nitriding. Both materials and method feed back into sustainable-nitrogen technologies: the iron nitrides here are catalyst candidates for greening ammonia — and therefore fertilizer — production, while the scattering approach transfers to nitrogen speciation and metal cycling in soils and plants.

Author

Greeshma Gadikota (Columbia University)

Co-authors

Mr Christopher Stoll (Cornell University) Dr Ivan Kuzmenko (Argonne National Laboratory) Dr Jan Ilavksy (Argonne National Laboratory) Prof. Luke Davis (Tufts University) Dr Sanya Mittal (Tufts University)

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