Yang C et al. (2019), Synthesis of nano-sized urchin-shaped LiFePO4 f...

ECB-ART-50722

RSC Adv 2019 May 03;924:13714-13721. doi: 10.1039/c9ra00897g.

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Synthesis of nano-sized urchin-shaped LiFePO4 for lithium ion batteries.

Yang C , Lee DJ , Kim H , Kim K , Joo J , Kim WB , Song YB , Jung YS , Park J .

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In this article, the facile synthesis of sea urchin-shaped LiFePO4 nanoparticles by thermal decomposition of metal-surfactant complexes and application of these nanoparticles as a cathode in lithium ion secondary batteries is demonstrated. The advantages of this work are a facile method to synthesize interesting LiFePO4 nanostructures and its synthetic mechanism. Accordingly, the morphology of LiFePO4 particles could be regulated by the injection of oleylamine, with other surfactants and phosphoric acid. This injection step was critical to tailor the morphology of LiFePO4 particles, converting them from nanosphere shapes to diverse types of urchin-shaped nanoparticles. Electron microscopy analysis showed that the overall dimension of the urchin-shaped LiFePO4 particles varied from 300 nm to 2 μm. A closer observation revealed that numerous thin nanorods ranging from 5 to 20 nm in diameter were attached to the nanoparticles. The hierarchical nanostructure of these urchin-shaped LiFePO4 particles mitigated the low tap density problem. In addition, the nanorods less than 20 nm attached to the edge of urchin-shaped nanoparticles significantly increased the pathways for electronic transport.

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References [+] :

Chi, Optimizing LiFePO₄@C core-shell structures via the 3-aminophenol-formaldehyde polymerization for improved battery performance. 2014, Pubmed

	Scheme 1. Synthesis illustration and procedure of spherical LiFePO4 nanoparticles (NS-LFP), urchin-shaped LiFePO4 (NU-LFP) nanoparticles, discrete urchin-shaped LiFePO4 nanoparticles (DNU-LFP), and circular urchin-shaped LiFePO4 nanoparticles (CNU-LFP).
	Fig. 1. TEM images of (a) NS-LFP; (b) NU-LFP, oleylamine and H3PO4 were injected at the end of the 1st aging at 200 °C; (c) DNU-LFP, only H3PO4 was injected at the end of the 1st aging at 200 °C; (d) CNU-LFP, 1.38 mmol of octadecylamine and 10.12 mmol of oleylamine were mixed with metal precursors, and only H3PO4 was injected at the end of the 1st aging at 200 °C and then aged for 3 h at 260 °C.
	Fig. 2. XRD characterization of (a) spherical LiFePO4 nanoparticles (NS-LFP) and (b) circular urchin-shaped LiFePO4 nanoparticles (NU-LFP).
	Fig. 3. (a) SEM image of nano urchin-shaped LiFePO4 nanoparticles (NU-LFP NPs), (b) and (c) HRTEM images of the NU-LFP NPs, and (d)fast Fourier transform images of NU-LFP NPs.
	Fig. 4. TEM images of urchin-shaped DNU-LFP nanoparticles obtained for the sample aliquots drawn from the solution undergoing 2nd aging step at 260 °C. Aged for (a) 30 min, (b) 40 min, (c) 50 min, (d) 1.5 h, (e) and (f) 2 h.
	Fig. 5. TEM images of (a) CNU-LFP, and (b) CNU-LFP annealed at 350 °C for 3 h with 4% hydrogen under argon atmosphere. (c) TGA data and (d) FT-IR of CNU-LFP.
	Fig. 6. Charge/discharge curves of the CNU-LFP cathode between 2.5 and 4.0 V (vs. Li/Li+) at a current rate of 0.05C.
	Fig. 7. Charge/discharge curves of (a) calcinated CNU-LFP cathode and (b) calcinated NU-LFP between 2.5 and 4.0 V (vs. Li/Li+) at a current rate of 0.05C. Cyclic performance of (c) calcinated CNU-LFP cathode and (d) calcinated NU-LFP at 0.05C.
	Fig. 8. Rate performance of calcinated CNU-LFP cathode.