한국결정성장학회지 (Journal of the Korean Crystal Growth and Crystal Technology)

  • 제21권1호
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  • Pages.15-20
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  • 2011
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  • 1225-1429(pISSN)
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  • 2234-5078(eISSN)
한국결정성장학회 (The Korea Association of Crystal Growth)
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LiFePO4와 Li4P2O7의 7Li MAS NMR 특성 연구

7Li MAS NMR studies of Li4P2O7 and LiFePO4 materials

  • 투고 : 2010.11.15
  • 심사 : 2011.01.07
  • 발행 : 2011.02.28
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초록

[ $^7Li$ ]Magic Angle Spinning(MAS) NMR Spectroscopy를 활용하여 $Li_4P_2O_7$와 $LiFePO_4$ 물질에서 $^7Li$ 핵의 NMR 특성 및 화합물 분자내의 국부적 구조 연구를 수행하였다. $Li_4P_2O_7$와 $LiFePO_4$ 물질 연구는 리튬이온전지에서 고체-전해질 경계상(SEI, solid-electrolyte interphase) 물질 연구를 위한 것이다. $Li_4P_2O_7$와 $LiFePO_4$ 분말은 고상합성법으로 제조하였다.$^7Li$MAS NMR 실험은 $27^{\circ}C$에서 $97^{\circ}C$의 영역에서 변온 실험을 수행하였으며 이는 주변 온도 변화 환경에서 $Li_4P_2O_7$ 물질 내의 Li 핵의 구조 변화를 관찰하기 위한 것이다. $^7Li$ MAS NMR 측정 결과 시료 온도가 $27^{\circ}C$에서 $97^{\circ}C$의 온도 분포 영역에서는 $Li_4P_2O_7$ 물질 내부의 Li 핵은 구조적으로 변화하지 않는 것이 확인되었다. 금번 실험을 통하여 $LiFePO_4$ 분말에 5.0 wt%이내로 포함되어있는 $Li_4P_2O_7$ 물질의 $^7Li$ MAS NMR 신호를 측정할 수 있는 측정 조건을 알았다.

[ $^7Li$ ]Magic Angle Spinning (MAS) NMR spectroscopy has been used to study the lithium local environments in $Li_4P_2O_7$ and$LiFePO_4$ materials. The purpose of this study was to know the structure of the solid electrolyte interphase (SEI) in lithium ion cells composed of $LiFePO_4$ as cathode material. $Li_4P_2O_7$ and $LiFePO_4$ were prepared by a solid-state reaction. The $^7Li$ MAS NMR experiments were carried out at variable temperatures in order to observe the local structure changes at the temperatures in $Li_4P_2O_7$ system. The $^7Li$ MAS NMR spectra of in $Li_4P_2O_7$ indicate that the lithium local environments in $Li_4P_2O_7$ were not changed in the temperature range between $27^{\circ}C$ and $97^{\circ}C$ Through this work, we confirmed that the small amount of $Li_4P_2O_7$ less than 5.0 wt% in $LiFePO_4$ could be clearly measured by the $^7Li$ MAS NMR spectroscopy at high spinning rate over than 11 kHz.

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