Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

Marca M. Doeff; Guoying Chen; Jordi Cabana; Thomas J. Richardson; Apurva Mehta; Mona Shirpour; Hugues Duncan; Chunjoong Kim; Kinson C. Kam; Thomas Conry

doi:10.3791/50594

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Method Article

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

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DOI:

10.3791/50594

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November 11th, 2013

Marca M. Doeff¹ , Guoying Chen¹ , Jordi Cabana¹^,² , Thomas J. Richardson¹ , Apurva Mehta³ , Mona Shirpour¹ , Hugues Duncan¹ , Chunjoong Kim¹ , Kinson C. Kam⁴ , Thomas Conry⁵

¹Environmental Energy Technologies Division, Lawrence Berkeley National Laboratory, ²Department of Chemistry, University of Illinois at Chicago, ³Stanford Synchrotron Radiation Lightsource, ⁴Haldor Topsøe A/S, ⁵PolyPlus Battery Company

Summary

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

Abstract

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g. changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g. on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

Introduction

Lithium ion batteries for consumer electronics presently command an $11 billion market worldwide (http://www.marketresearch.com/David-Company-v3832/Lithium-Ion-Batteries-Outlook-Alternative-6842261/) and are the premier choice for emerging vehicular applications such as plug-in hybrid electric vehicles (PHEVs) and electric vehicles (EVs). Analogs to these devices utilizing sodium ions rather than lithium are in earlier stages of development, but are considered attractive for large scale energy storage (i.e. grid applications)....