A system for performing simultaneous in situ atomic force microscopy/optical microscopy measurements on electrode materials for lithium-ion batteries

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Abstract
An atomic force microscope (AFM) equipped with an optical charge coupled device camera has been placed in an Ar filled glovebox for the purpose of studying the change in morphology of electrode materials as they react with lithium. In order to minimize noise induced by vibration, the AFM is mounted on granite blocks suspended from the ceiling of the glovebox by a combination of flexible rubber cords and metal springs. The AFM, which is equipped with an environmental chamber surrounding the sample, is then enclosed in a specially constructed draft shield that allows the circulation of Ar gas by the purification system during imaging. A special electrochemical cell was constructed to hold the working electrode under study. Repeated imaging with little drift is possible while electrodes are reacted with lithium for periods of many days. Examples of measurements made by this device will be given for the case of lithium alloying with sputter-deposited Si–Sn thin films. The optical and AFM images obtained as a function of lithium content in the films are assembled into time-lapsed “movies” showing the evolution of the morphology of the sample along with the corresponding electrochemistry. These movies are available for download through the Electronic Physics Auxiliary Publication Service (EPAPS).