LiFePO4/C has been successfully synthesized using surfactant-assisted solid-state reaction method to investigate the effects of non-polar solvents on structural properties and electrochemical performance. Petroleum jelly, oleic acid, and sucrose were used as non-polar solvents, surfactants and carbon sources. The ratio of petroleum jelly and oleic acid were 0.5:1 (LFP A), 1:1 (LFP B), and 2:1 (LFP C). The XRD, FE-SEM, and HR-TEM results show that adding petroleum jelly in LFP C enhances crystallinity and improves the morphology of nanoplates in LiFePO4 material. The EDS and Raman Spectroscopy tests show that the higher addition of petroleum jelly increases carbon percentage and carbon layer defects. The highest Li-ion diffusion coefficient was calculated by LFP C of 4.21 × 10– 15 cm2. s−1. Furthermore, the highest discharge test results at 0.1 C of LFP A, LFP B, and LFP C were 125 mAh.g−1, 103 mAh.g−1, and 144 mAh.g−1, respectively. However, C-rate performance shows that the specific capacity of LFP A, LFP B, and LFP C at 5 C were 74 mAh.g−1, 35 mAh.g−1, and 59 mAh.g−1, respectively. The cyclability test results showed that LFP A capacity retention after testing for 100 cycles was better than LFP C, and the lowest stability was obtained by LFP B. The addition of petroleum jelly improved the performance of LiFePO4/ C but resulted in excess carbon in active material which decreased battery stability and specific capacity at high C-rate. Our results suggest that non-polar solvents can be added to LiFePO4/ C synthesis to improve electrochemical performance but less carbon chains must be chosen.

개량된 MA법으로 합성된 LiFe(PO4)/C에 대해 X-선 회절분석을 실시하여 리트벨트법에 의해 결정학적 연구를 수행하였다. 리트벨트 계산 결과 리트벨트 R 지수 값은 Rp=8.14%, Rwp=11.1%, Rexp=9.09%, RB=3.88%, S (GofF, Goodness of fit) = 1.2으로 계산이 잘 이루어졌음을 알 수 있다. LiFePO4/C는 공간군 Pnma를 가지며, 격자상수 값은 a = 10.3229(3)a, b = 6.0052(2) a, c = 4.6939(1) a이고 체적값은 V = 290.98(1) a3으로 기존 다른 합성법의 연구결과와 잘 일치한다. 분말 입자는 고순도를 가지고 나노 크기(65~90nm)로 기존 MA법보다 상대적으로 미세하고 균질도가 향상되었다. 따라서 개량된 MA법은 상업용 리튬 2차 전지의 양극물질 생산을 위한 우수한 제조법으로 판단된다.