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A series of non-stoichiometric potassium rhodate single-crystals KxRhO2 (x=0.72,0.64,0.63,0.55) have been synthesized by the spontaneous nucleation under different growth conditions and subsequent chemically de-intercalation.The crystal structure/structural evolution,morphology/composition and microstructure of these samples were characterized by X-ray diffraction,scanning electron microscopy/energy dispersive spectroscopy and transmission electron microscopy.