Combined operando X-ray diffraction–electrochemical impedance spectroscopy detecting solid solution reactions of LiFePO4 in batteries

Michael Hess (), Tsuyoshi Sasaki (), Claire Villevieille and Petr Novák
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Michael Hess: Paul Scherrer Institute, Electrochemical Energy Storage Section
Tsuyoshi Sasaki: Paul Scherrer Institute, Electrochemical Energy Storage Section
Claire Villevieille: Paul Scherrer Institute, Electrochemical Energy Storage Section
Petr Novák: Paul Scherrer Institute, Electrochemical Energy Storage Section

Nature Communications, 2015, vol. 6, issue 1, 1-9

Abstract: Abstract Lithium-ion batteries are widely used for portable applications today; however, often suffer from limited recharge rates. One reason for such limitation can be a reduced active surface area during phase separation. Here we report a technique combining high-resolution operando synchrotron X-ray diffraction coupled with electrochemical impedance spectroscopy to directly track non-equilibrium intermediate phases in lithium-ion battery materials. LiFePO4, for example, is known to undergo phase separation when cycled under low-current-density conditions. However, operando X-ray diffraction under ultra-high-rate alternating current and direct current excitation reveal a continuous but current-dependent, solid solution reaction between LiFePO4 and FePO4 which is consistent with previous experiments and calculations. In addition, the formation of a preferred phase with a composition similar to the eutectoid composition, Li0.625FePO4, is evident. Even at a low rate of 0.1C, ∼20% of the X-ray diffractogram can be attributed to non-equilibrium phases, which changes our understanding of the intercalation dynamics in LiFePO4.

Date: 2015
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DOI: 10.1038/ncomms9169

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