Crystal Growth Behavior of LiFePO4 in Microwave-Assisted Hydrothermal Condition: From Nanoparticle to Nanosheet

By using microwave-assisted hydrothermal crystallization approach, LiFePO4 nanoparticles have been synthesized in several minutes without the use of any organic reducing agent and argon protection. The crystal structure and lattice parameters have been analyzed by using the X-ray diffraction patterns (XRD) and Rietveld refined analysis, and the full width at half-maximum (FWHM) of the characteristic peaks. A preferential orientation of crystal growth occurs upon microwave hydrothermal field. The SEM and TEM images show that the LiFePO4 crystals present a change from nanoparticle to nanosheet with the increasing reaction time from 5 to 20 min. All the samples present a couple of redox peaks in their CV profiles. The peak pair corresponds to the charge/discharge reaction of the Fe3+/Fe2+ redox couple, and evidencing the absence of electroactive iron impurities. Because of the LiFePO4 samples prepared without any carbon, the initial charge/discharge capacities and cycleability of absolutely are affected by the crystal structure which is controlled by the microwave irradiation condition. The relation among the microwave reaction condition, crystal morphology, and the electrochemical properties are presented and discussed in the electrochemical test.