Electrochemical (de)lithiation of silver ferrite and composites: mechanistic insights from ex situ, in situ, and operando X-ray techniques

Durham, Jessica L.; Brady, Alexander B.; Cama, Christina A.; Bock, David C.; Pelliccione, Christopher J.; Zhang, Qing; Ge, Mingyuan; Li, Yue Ru; Zhang, Yiman; Yan, Hanfei; Huang, Xiaojing; Chu, Yong; Takeuchi, Esther S.; Takeuchi, Kenneth J.; Marschilok, Amy C.

doi:10.1039/C7CP04012A

Title: Electrochemical (de)lithiation of silver ferrite and composites: mechanistic insights from ex situ, in situ, and operando X-ray techniques

Journal Article · Wed Aug 02 00:00:00 EDT 2017 · Physical Chemistry Chemical Physics. PCCP

DOI:https://doi.org/10.1039/C7CP04012A· OSTI ID:1376184

Durham, Jessica L. ^[1]; Brady, Alexander B. ^[2]; Cama, Christina A. ^[1]; Bock, David C. ^[3]; Pelliccione, Christopher J. ^[3]; Zhang, Qing ^[2]; Ge, Mingyuan ^[4]; Li, Yue Ru ^[1]; Zhang, Yiman ^[1]; Yan, Hanfei ^[4]; Huang, Xiaojing ^[4]; Chu, Yong ^[4];

^[5]; Takeuchi, Kenneth J. ^[6];

^[6]

Stony Brook Univ., NY (United States). Dept. of Chemistry
Stony Brook Univ., NY (United States). Dept. of Materials Science and Engineering
Brookhaven National Lab. (BNL), Upton, NY (United States). Energy Sciences Directorate
Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
Stony Brook Univ., NY (United States). Dept. of Chemistry; Stony Brook Univ., NY (United States). Dept. of Materials Science and Engineering; Brookhaven National Lab. (BNL), Upton, NY (United States). Energy Sciences Directorate
Stony Brook Univ., NY (United States). Dept. of Chemistry; Stony Brook Univ., NY (United States). Dept. of Materials Science and Engineering

Here, the structure of pristine AgFeO₂ and phase makeup of Ag_0.2FeO1.6 (a one-pot composite comprised of nanocrystalline stoichiometric AgFeO₂ and amorphous γ-Fe₂O₃ phases) was investigated using synchrotron x-ray diffraction. A new stacking-fault model was proposed for AgFeO2 powder synthesized using the co-precipitation method. The lithiation/de-lithiation mechanisms of silver ferrite, AgFeO₂ and Ag_0.2FeO_1.6 were investigated using ex-situ, in-situ, and operando characterization techniques. An amorphous γ-Fe₂O₃ component in the Ag_0.2FeO_1.6 sample is quantified. Operando XRD of electrochemically reduced AgFeO₂ and Ag_0.2FeO_1.6 composites demonstrated differences in the structural evolution of the nanocrystalline AgFeO₂ component. As complimentary techniques to XRD, ex-situ x-ray Absorption Spectroscopy (XAS) provided insight into the short-range structure of the (de)lithiated nanocrystalline electrodes, and a novel in-situ high energy x-ray fluorescence nanoprobe (HXN) mapping measurement was applied to spatially resolve the progression of discharge. Based on the results, a redox mechanism is proposed where the full reduction of Ag⁺ to Ag0 and partial reduction of Fe³⁺ to Fe²⁺ occur on reduction to 1.0 V, resulting in a Li_1+yFe^IIIFe^IIyO₂ phase. The Li_1+yFe^IIIFe^IIyO₂ phase can then reversibly cycle between Fe³⁺ and Fe²⁺ oxidation states, permitting good capacity retention over 50 cycles. In the Ag_0.2FeO_1.6 composite, a substantial amorphous γ-Fe₂O₃ component is observed which discharges to rock salt LiFe₂O₃ and Fe⁰ metal phase in the 3.5 – 1.0 V voltage range (in parallel with the AgFeO₂ mechanism), and reversibly reoxidizes to a nanocrystalline iron oxide phase.

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Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: SC0012704; AC02-06CH11357

OSTI ID:: 1376184

Report Number(s):: BNL-114168-2017-JA; PPCPFQ

Journal Information:: Physical Chemistry Chemical Physics. PCCP, Vol. 19, Issue 33; ISSN 1463-9076

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 9 works

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