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The paper presents a comprehensive study of the physicochemical and electrochemical properties of a new nano-microporous non-woven composite separation material for a lithium-ion battery based on nano- and microfibers of polyvinylidene fluoride (PVDF) and its copolymer with polytetrafluoroethylene (PTFE), obtained by capillary-less electrospinning. A technique for the synthesis of separation material was developed, and the composition of the polymeric solution and the electrospinning conditions were optimized to produce polymer nano-microfibers with the required physicochemical characteristics. The optimal synthesis conditions for the separation material were determined. Higher porosity of the separation material and increased wettability in the most common electrolyte compositions contribute to the higher conductivity of the obtained separation material in comparison with the widely used commercial separation materials based on polypropylene (PP). The working characteristics of the separation material were studied in laboratory half-cells with a working electrode based on Li4Ti5O12, as well as a lithium metal counter electrode and a reference electrode. Charge-discharge tests of cells were performed in a wide range of variation of currents: From 0.1 to 25 C. A decrease in the total polarization of the working electrode and an increase in the cycled capacity at comparable currents in comparison with a cell with a PP-based separator were noted. The state of the electrodes and the separator in the cell was monitored using electrochemical impedance spectroscopy: The polarization resistances of the electrodes in different frequency ranges were determined, and the diffusion coefficient of lithium ions in the Li4Ti5O12 electrode was estimated in various lithiation states and at different stages of electrochemical tests, which were in the interval of 10−10 to 10−9 cm2·s−1.

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