Raman spectra of isolated single particles of technical grade LiMn2O4 (mean diam ca. 10 μm) embedded in Au foils were recorded in situ in 1 M LiPF6 in ethylene carbonate/dimethyl carbonate (2:1 w/w) solutions using a Raman microscope. Data collected under steady state as a function of applied potential were in excellent agreement with those reported for the material using other approaches. In addition, the rather high signal to noise ratios made it possible, for the first time, to monitor in real time the spectral properties of individual particles under transient conditions during a voltammetric scan. Extensions of this novel in situ measurement strategy are expected to allow the electrical state of particles incorporated into electrodes in battery-type environments to be determined spectroscopically both with temporal and spatial resolution, enabling in certain instances direct comparisons to be made with predictions based on theoretical modeling.
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