Sintering inhibition enables hierarchical porosity with extreme resistance to degradation during redox cycling of Fe-Mo foams

Jacob B. Mack; Samuel M. Pennell; David C. Dunand

doi:10.1016/j.actamat.2023.119015

Sintering inhibition enables hierarchical porosity with extreme resistance to degradation during redox cycling of Fe-Mo foams

Jacob B. Mack^*, Samuel M. Pennell, David C. Dunand

^*Corresponding author for this work

Materials Science and Engineering

Research output: Contribution to journal › Article › peer-review

5 Scopus citations

Abstract

High-temperature (800 ºC) steam-hydrogen redox cycling, relevant to grid-scale energy storage, is studied for iron-based freeze-cast lamellar foams. In contrast to previously studied Fe, Fe-Ni, and Fe-Co foams that rapidly degrade, Fe-25Mo foams feature a much-enhanced structural damage resistance. Utilizing in-situ x-ray diffraction, microscopy, and x-ray tomography, strong sintering inhibition is observed in Fe-Mo foams, creating a hierarchically porous lamellar structure. This leads to (i) wide channels between lamellae, enabling high macroscopic porosity (∼78%) which can accommodate gas flow as well as volumetric expansion without lamellar contact, and (ii) microporosity within lamellae, providing additional free volume to accommodate expansion during oxidation, limiting both swelling of the lamellae and the formation of Kirkendall pores. These combined effects enable a near-complete reversibility of the microstructure during cycling, preventing damage produced via internal lamellar buckling, cracking, contacting and sintering, with a remarkably high porosity (65%) remaining after 50 consecutive redox cycles.

Original language	English (US)
Article number	119015
Journal	Acta Materialia
Volume	254
DOIs	https://doi.org/10.1016/j.actamat.2023.119015
State	Published - Aug 1 2023

Funding

This research was funded by the US National Science Foundation under grant CMMI-2015641. Experiments and characterization made use of the Materials Characterization and Imaging Facility, the NUANCE Center (supported by SHyNE under NSF ECCS-1542205, MRSEC under NSF DMR-1720139, the International Institute for Nanotechnology, the Keck Foundation, and the State of Illinois), and the IMSERC X-Ray facility (supported by SHyNE under NSF ECCS-2025633) at Northwestern University (NU). Microtomography was performed at the DuPont-Northwestern-Dow Collaborative Access Team (DND-CAT) located at Sector 5 of the Advanced Photon Source (APS). DND-CAT is supported by Northwestern University, The Dow Chemical Company, and DuPont de Nemours, Inc. This research used resources of the Advanced Photon Source, a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under Contract No. DE-AC02-06CH11357.

Keywords

Freeze-casting
Hydrogen
Porosity
Redox cycling
Sintering

ASJC Scopus subject areas

Electronic, Optical and Magnetic Materials
Ceramics and Composites
Polymers and Plastics
Metals and Alloys

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10.1016/j.actamat.2023.119015

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title = "Sintering inhibition enables hierarchical porosity with extreme resistance to degradation during redox cycling of Fe-Mo foams",

abstract = "High-temperature (800 ºC) steam-hydrogen redox cycling, relevant to grid-scale energy storage, is studied for iron-based freeze-cast lamellar foams. In contrast to previously studied Fe, Fe-Ni, and Fe-Co foams that rapidly degrade, Fe-25Mo foams feature a much-enhanced structural damage resistance. Utilizing in-situ x-ray diffraction, microscopy, and x-ray tomography, strong sintering inhibition is observed in Fe-Mo foams, creating a hierarchically porous lamellar structure. This leads to (i) wide channels between lamellae, enabling high macroscopic porosity (∼78%) which can accommodate gas flow as well as volumetric expansion without lamellar contact, and (ii) microporosity within lamellae, providing additional free volume to accommodate expansion during oxidation, limiting both swelling of the lamellae and the formation of Kirkendall pores. These combined effects enable a near-complete reversibility of the microstructure during cycling, preventing damage produced via internal lamellar buckling, cracking, contacting and sintering, with a remarkably high porosity (65%) remaining after 50 consecutive redox cycles.",

keywords = "Freeze-casting, Hydrogen, Porosity, Redox cycling, Sintering",

author = "Mack, {Jacob B.} and Pennell, {Samuel M.} and Dunand, {David C.}",

note = "Publisher Copyright: {\textcopyright} 2023 Acta Materialia Inc.",

year = "2023",

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doi = "10.1016/j.actamat.2023.119015",

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AU - Mack, Jacob B.

AU - Pennell, Samuel M.

AU - Dunand, David C.

PY - 2023/8/1

Y1 - 2023/8/1

N2 - High-temperature (800 ºC) steam-hydrogen redox cycling, relevant to grid-scale energy storage, is studied for iron-based freeze-cast lamellar foams. In contrast to previously studied Fe, Fe-Ni, and Fe-Co foams that rapidly degrade, Fe-25Mo foams feature a much-enhanced structural damage resistance. Utilizing in-situ x-ray diffraction, microscopy, and x-ray tomography, strong sintering inhibition is observed in Fe-Mo foams, creating a hierarchically porous lamellar structure. This leads to (i) wide channels between lamellae, enabling high macroscopic porosity (∼78%) which can accommodate gas flow as well as volumetric expansion without lamellar contact, and (ii) microporosity within lamellae, providing additional free volume to accommodate expansion during oxidation, limiting both swelling of the lamellae and the formation of Kirkendall pores. These combined effects enable a near-complete reversibility of the microstructure during cycling, preventing damage produced via internal lamellar buckling, cracking, contacting and sintering, with a remarkably high porosity (65%) remaining after 50 consecutive redox cycles.

AB - High-temperature (800 ºC) steam-hydrogen redox cycling, relevant to grid-scale energy storage, is studied for iron-based freeze-cast lamellar foams. In contrast to previously studied Fe, Fe-Ni, and Fe-Co foams that rapidly degrade, Fe-25Mo foams feature a much-enhanced structural damage resistance. Utilizing in-situ x-ray diffraction, microscopy, and x-ray tomography, strong sintering inhibition is observed in Fe-Mo foams, creating a hierarchically porous lamellar structure. This leads to (i) wide channels between lamellae, enabling high macroscopic porosity (∼78%) which can accommodate gas flow as well as volumetric expansion without lamellar contact, and (ii) microporosity within lamellae, providing additional free volume to accommodate expansion during oxidation, limiting both swelling of the lamellae and the formation of Kirkendall pores. These combined effects enable a near-complete reversibility of the microstructure during cycling, preventing damage produced via internal lamellar buckling, cracking, contacting and sintering, with a remarkably high porosity (65%) remaining after 50 consecutive redox cycles.

KW - Freeze-casting

KW - Hydrogen

KW - Porosity

KW - Redox cycling

KW - Sintering

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Sintering inhibition enables hierarchical porosity with extreme resistance to degradation during redox cycling of Fe-Mo foams

Abstract

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Keywords

ASJC Scopus subject areas

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