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Ambient synthesis, characterization, and electrochemical activity of LiFePO4 nanomaterials derived from iron phosphate intermediates

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Abstract

LiFePO4 materials have become increasingly popular as a cathode material due to the many benefits they possess including thermal stability, durability, low cost, and long life span. Nevertheless, to broaden the general appeal of this material for practical electrochemical applications, it would be useful to develop a relatively mild, reasonably simple synthesis method of this cathode material. Herein, we describe a generalizable, 2-step methodology of sustainably synthesizing LiFePO4 by incorporating a template-based, ambient, surfactantless, seedless, U-tube protocol in order to generate size and morphologically tailored, crystalline, phase-pure nanowires. The purity, composition, crystallinity, and intrinsic quality of these wires were systematically assessed using transmission electron microscopy (TEM), high-resolution TEM (HRTEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), selected area electron diffraction (SAED), energy dispersive analysis of X-rays (EDAX), and high-resolution synchrotron XRD. From these techniques, we were able to determine that there is an absence of any obvious defects present in our wires, supporting the viability of our synthetic approach. Electrochemical analysis was also employed to assess their electrochemical activity. Although our nanowires do not contain any noticeable impurities, we attribute their less than optimal electrochemical rigor to differences in the chemical bonding between our LiFePO4 nanowires and their bulk-like counterparts. Specifically, we demonstrate for the first time experimentally that the Fe-O3 chemical bond plays an important role in determining the overall conductivity of the material, an assertion which is further supported by recent “first-principles” calculations. Nonetheless, our ambient, solution-based synthesis technique is capable of generating highly crystalline and phase-pure energy-storage-relevant nanowires that can be tailored so as to fabricate different sized materials of reproducible, reliable morphology.

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  1. Jason A. Graetz

    Present address: Sensors and Materials Laboratory, HRL Laboratories, LLC, 3011 Malibu Canyon Road, Malibu, CA, 90265-4797, USA

Authors and Affiliations

  1. Department of Chemistry, State University of New York at Stony Brook, Stony Brook, NY, 11794-3400, USA

    Jonathan M. Patete, Megan E. Scofield, Christopher Koenigsmann, Yiman Zhang, Amy C. Marschilok, Xiaoya Wang, Lei Wang & Stanislaus S. Wong

  2. Condensed Matter Physics and Materials Sciences Department, Building 480, Brookhaven National Laboratory, Upton, NY, 11973, USA

    Vyacheslav Volkov, Jinkyu Han, Yimei Zhu & Stanislaus S. Wong

  3. Department of Materials Science and Engineering, State University of New York at Stony Brook, Stony Brook, NY, 11794-2275, USA

    Amy C. Marschilok

  4. Sustainable Energy Technologies Department, Building 815, Brookhaven National Laboratory, Upton, NY, 11973, USA

    Xiaoya Wang, Feng Wang & Jason A. Graetz

  5. National Synchrotron Light Source II, Building 741, Brookhaven National Laboratory, Upton, NY, 11973, USA

    Jianming Bai

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Patete, J.M., Scofield, M.E., Volkov, V. et al. Ambient synthesis, characterization, and electrochemical activity of LiFePO4 nanomaterials derived from iron phosphate intermediates. Nano Res. 8, 2573–2594 (2015). https://doi.org/10.1007/s12274-015-0763-5

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