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International audienceThis study demonstrates the unique capabilityof infrared near-field nanoscopy combined with Fouriertransform infrared spectroscopy to map phase distributionsin microcrystals of LixFePO4, a positive electrode material forLi-ion batteries. Ex situ nanoscale IR imaging provides directevidence for the coexistence of LiFePO4 and FePO4 phases inpartially delithiated single-crystal microparticles. A quantitativethree-dimensional tomographic reconstruction of the phasedistribution within a single microcrystal provides new insightsinto the phase transformation and/or relaxation mechanism,revealing a FePO4 shell surrounding a diamond-shaped LiFePO4 inner core, gradually shrinking in size and vanishing upondelithiation of the crystal. The observed phase propagation pattern supports recent functional models of LiFePO4 operationrelating electrochemical performance to material design. This work demonstrates the remarkable potential of near-field opticaltechniques for the characterization of electrochemical materials and interfaces

IR Near-Field Spectroscopy and Imaging of Single LixFePO4 Microcrystals