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1 Jurnal f the Krean Electrchemical Sciety Vl. 1, N. 1, 009, t gq mw-j.o 0 š ¼ Á yá x Á w yw œw y l w» w»» Á w ( :009 9 k) Imprvement f High-Temperature Perfrmance f Cathde by Surface Cating Gil-Wn Lee, Jng-Hwa Lee, Ji Hen Ryu, and Seung M. Oh* Department f Chemical and Bilgical Engineering and Research Center fr Energy Cnversin & Strage, Seul Natinal University, Seul 151-7, Krea Graduate Schl f Knwledge-Based Technlgy and Energy, Krea Plytechnic University, Siheung, Gyenggi, 9-793, Krea (Received January 30, 009 : Accepted February 9, 009) p y v y (, LMO) t ITO(indium tin xide) gqw, š (55 C) j p w. Á x, ITOƒ gq LMO t š Áš w ww v x š, v w w x (plarizatin) w w. ù, ITOƒ ml% gq LMO y w, w wƒ w š ü w w x w x w. w, ITOƒ gq ƒ gq LMO w j w. Ÿ» w ITOƒ gq LMO t v x w y w. ITO gq LMO p j w, w j v x ITO» ƒ j w. Abstract : An indium-tin xide (ITO) cated spinel manganese xide (, LMO) is prepared and its high-temperature (55 C) cycle perfrmance and rate capability are examined. A severe electrlyte decmpsitin and film depsitin is bserved n the un-cated cathde, which leads t a significant electrde plarizatin and capacity fading. Such an electrde plarizatin is, hwever, greatly reduced fr the ITO-cated (> ml%) LMO cathde, which leads t an imprved cycle perfrmance. This can be ratinalized by a suppressin f electrlyte decmpsitin, which is in turn indebted t a decrease in the direct cntact area between LMO and electrlyte. The suppressin f film depsitin n the ITO-cated LMO cathde is cnfirmed by infra-red spectrscpy. The rate capability is als imprved by the surface cating, which may be resulted frm a suppressin f resistive film depsitin and high electric cnductivity f ITO itself. Keywrds : Lithium-in batteries, Cathde,, Indium-tin xide (ITO), Surface catingu * seungh@snu.ac.kr 81

2 8 J. Krean Electrchem. Sc., Vl. 1, N. 1, v ƒ š, ey, w w ƒ š. ù 1-3) w š š w w. p š ) Mn w w w» w ƒ j š. 5) V w ƒ» š. Tarascn v ü Li Mn ä(catin mixing) w ƒ, x.5 V (vs. Li/Li + ) y/y vj w. 6-7) Dahn v w w w v ü w w š, 3.3 V sk (vltage plateau) w. 8-9) Yshi (tw-phase reactin) w w ƒ ù š w. w 10) Thackeray Mn 3+ ³ y (disprprtinatin) w Mn + /Mn y / y š w y +»w š w. š ) Oh Mn w w y (plarizatin) ƒ w ƒ ù š w. 11) w v w w» w Mn eyw LiM y Mn -y (M = Li, B, Al, Cr, C, Ni) w w w y g. w 1-13) w t p yƒ j w e, t w» y j w k š. Al O 3, ZrO, ZnO, C 3 y gqw ƒ w k ƒ y w. 1-17) wù w w v x, x w» w, z ITO (indium tin xide, SnO -dped In O 3 )ƒ gq w. ITO gq w w/v x / y»yw d, Ÿ» w w. w ITO» ƒ 10 ~10 Scm 1 w, ITO gq p w w.. x ITOƒ gq w w» w, In Sn ƒ 9:1 In(NO 3 ) 3 5H O(Aldrich, 99.9%) Sn(Ot-Bu) (Aldrich, %) ethanl ITOcating w.» (Merck C.) k z w. ITO w 1,, 3, ml%ƒ w. z»(rtary evapratr) ethanl w z, 150 C 30 w ethanl w. z ITO x w 500 C 6 w. w w ITOƒ gq. Fig. 1 w ùkü. t xk y w» w JEOL(Mdel JSM-6700F) x x (field-emissin scanning electrn micrscpe, FE-SEM) w, gq Ì w» w Philips Electrn Optics(mdel CM-0) n x (transmissin electrn micrscpe, TEM) w. ITOƒ gq y w w w. y, (Super P) š w (ply(vinyledienfluride), PVdF) 9:: w z, NMP(1-methyl-- Fig. 1. Schematic diagram fr the preparatin f ITOcated pwder.

3 한국전기화학회지, 제 1권, 제 1 호, 009 pyrrlidinne, Aldrich) 를 분산매로 사용하여 hmgenizer (Iuchi c. mdel CM-00)를 이용하여 혼합한 후 슬러리를 제조하였다. 이를 Al fil에 film cater(tester Sangy C. mdel PI-110) 를 이용하여 0~50 μm 정도의 두께로 도포한 후, 10 C에서 건조시켜 극판을 제조하였다. 이 렇게 제조한 극판을 rll press(kum-mc Machinery C.) 를 이용하여 30~35 μm 정도의 두께로 압착한 후, 지름 1.1cm 의 punch로 뚫어서 양극으로 사용하였다. 음극으로 Li fil(cyprus Fte Mineral C.)을, 전해질로는 EC (ethylene carbnate) + DMC (dimethyl carbnate) (1 : v/)/1.0 M LiPF 를, 분리막으로 다공질의 PP (plyprpylene) 을 사용하여, CR03 형태의 cin-cell (Hshen C. Japan) 을 이용하여 극셀을 아르곤이 채 워진 드라이 박스에서 제조한 후에 고온(55 C)에서 전 기화학 실험을 수행하였다. 전지의 충방전 실험은 정전류 방식(CC, cnstant current) 으로 0.5 macm (C/ rate)의 정전류를 충전과 방전 시에 인가하였다. 속도특성 조사를 위하여 0. macm (C/5 rate)~3 macm (3C rate) 범위에서 전류밀도를 변화시켰다. 방전(환원) cut-ff 전압은 3.V (vs. Li/Li ) 로, 충전(산화) cut-ff 전압은.3 V (vs. Li/Li )로 각각 고정하였다. 충방전 실험은 Wnatec(Mdel WBC-3000) 사의 정전류/정전위 제어가 가능한 충방전기를 이용하였다. 충방전 후 전해질 분해반응으로 인하여 양극 활물질 표면에 생성되는 피막의 상태를 확인하기 위하여, Bmen사 (Mdel DA 8)의 적외선분광기(Furier-transfrm infrared spectrmeter, FT-IR)를 이용하였다. 시료는 충방전 전후의 전지를 드라이 박스 내에서 분해하고 진공오븐에서 1시간 건조한 후에, KBr 분말과 시료의 비가 100 : 1가 되도록 혼합한 후 pellet으로 제조하여 측정하였다 결과 및 고찰 Fig. 는 ITO가 LiMn O 의 표면에 코팅 되었음을 확인 하기 위하여 FE-SEM 사진을 촬영한 결과를 나타낸 것이다. Fig. (a)와 (b)에서 알 수 있듯이 LiMn O 입자는 거친 표면을 가지고 있다. Fig. (c)와 (d)는 ITO가 코팅된 LiMn O 입자의 사진으로, 동일한 배율로 촬영한 Fig. (b)와 (d)를 비교하였을 때, 코팅된 입자의 경우 크기가 더 큰 입자들이 LiMn O 표면에 분포하고 있어 Fig.. FE-SEM images f the sample pwders: (a) and (b); LiMn O, and (c) and (d); ml% ITO-cated LiMn O.

4 8 J. Krean Electrchem. Sc., Vl. 1, N. 1, 009 Fig. 3. TEM images f the sample pwders: (a); LiMn O and (b); ml% ITO-cated LiMn O. Fig. 5. Rate capability bserved with Li/LiMn O and Li/ITO-cated LiMn O cells at 55 C. The C-rate is indicated in the inset. LiMn O 의 전기 전도도는 10 Scm 정도이나, ITO는 10 ~10 Scm 로 높은 전기전도도를 가지고 있다. ITO로 LiMn O 를 코팅함으로써, 일반적인 금속산화물의 코팅 1 1 효과뿐만 아니라 전자전달이 유리해질 수 있기 때문에 전극 의 속도특성에서도 좋은 효과를 기대할 수 있다. LiMn O 와 ITO가 코팅된 LiMn O 를 양극 활물질로 이용하여 정 전류방식으로 고온(55 C)에서 충방전 속도를 변화하며 충방전 실험을 수행한 결과 (Fig. 5), 코팅하지 않은 LiMn O 는 0. C에 비해 3 C일 경우 8%의 방전 용량을 보인 반면, ml% ITO가 코팅된 경우는 8%의 성능을 유지하였다. 코팅된 ITO의 양에 따라 비교해보면, 1ml%의 ITO가 코팅된 경우는 0. C에 비해 3 C일 때 66%의 성능만 을 유지했지만 ~ ml%의 경우는 모두 8% 이상의 성능을 유지하였다. 하지만, ITO의 코팅양이 증가하게 되 면 전극의 무게당 용량이 감소하므로, ml%의 ITO를 코팅하는 것이 최적이라 할 수 있다. 이와 같은 ITO의 코 팅에 따른 속도특성의 향상은 먼저 ITO의 높은 전기 전 도도에 기인한다고 설명할 수 있으나, 후에 제시할 저항이 큰 피막형성의 억제라는 측면에서도 설명이 가능하다. LiMn O 와 ITO가 코팅된 LiMn O 양극에서 전해질 분해 정도를 비교하기 위해서, 정전류 정전압(cnstant current/cnstant vltage, CC/CV) 충방전 실험을 수 행하였다. 정전류로.3 V까지 충전한 후,.3 V에 머무 르는 시간을 0, 6, 1시간으로 변화시켜 전해질의 분해 정도를 조절하면서 충방전에 따른 용량감소를 관찰하 였다. 이렇게 실험을 한 이유는 전해질 분해가.3 V에서 가장 심하다는 가정이 가능하기 때문이다. Fig. 6에서 보듯이, 코팅되지 않은 LiMn O 는 정전압(.3 V) 충전 시간이 길어질수록 용량감소가 크게 증가되었으나, ITO가 코팅된 LiMn O 는 정전압 충전 시간이 길어져도 용량 저하가 거의 없었다. 전해질 분해와 피막형성, 그리고 Fig.. Discharge capacity bserved with Li/LiMn O and Li/ITO-cated LiMn O cells at 55 C with 0.5 C-rate accrding t the cycle number. ITO가 코팅되었음을 유추할 수 있다. 또한 ITO가 LiMn O 입자표면의 대부분을 코팅하고 있음을 알 수 있다. 코팅된 층의 두께와 모양을 확인한 TEM 사진을 Fig. 3에 나타내었다. 사진에서 보듯이, 다소 불규칙적이나 LiMn O 입자 표면에 ITO가 50 nm정도로 코팅되어 있음을 확인할 수 있다. Fig. 에 코팅하지 않은 LiMn O 와 ITO가 코팅된 LiMn O 의 사이클 성능을 비교하였다. Fig. 에 제시한 결과는 초기 두 사이클은 전극의 안정화를 위하여 0. C 조건에서 충방전한 후, 3번째 사이클부터 0.5 C 조건으로 100회 충방전을 수행하였을 때 사이클에 따른 방전용 량을 비교한 그래프이다. 100회 충방전 하였을 때, 코팅되지 않은 경우는 초기용량의 68%를 유지한 반면, ~ ml% ITO로 코팅한 경우는 83%를 유지하고 있다. 즉, ITO로 표면을 코팅한 경우 가역성이 향상됨을 확인할 수 있다. 그러나 ml% 이상으로 코팅한 경우에 코팅 양에 따른 사이클 특성의 차이는 크지 않음을 알 수 있다.

5 w»ywz, 1«, 1 y, Fig. 6. Cycle perfrmance bserved at 55 C: (a); Li/ and (b); Li/ ml% ITO-cated cell. The charging was made at a cnstant current (C/ rate) frm 3. t.3 V and at cnstant vltage (.3 V) fr 0 h, 6 h and 1 h, whereas the discharging was made at a cnstant current (C/ rate) frm.3 t 3. V. Fig. 7. The charge/discharge vltage prfiles bserved at 55 C: (a); Li/ and (b); Li/ ml% ITO-cated cell. The charge-discharge cnditin was the same as fr Fig. 6. The 3 rd and 50 th cycles are represented. Nte the large electrde plarizatin at 50 th cycle fr the Li/ cell (a). x y y w» w Fig š ùkü. gq.3 V ¼ x j ƒw. Fig. 7(a) 3 w 50 j š ƒ j. ù, ITOƒ gq 50 j x w. w l, š w,» Mn w x x w w w., Fig. 7, 50 j ƒ w l Li k ƒ óù k cut-ff w w w. w, w w w w. ù, ITO gqw, x w x w. ü w ƒ w x w w w v x» w y w» w, z t k Ÿ» w (Fig. 8). Aurbach 700, 850, 900, 100, 1300 š 100 cm w PVdF 1 w šw. 18) Fig. 8 w rp w q PVdF w y w. w 100z z rp, O-H stretching (300~3600 cm 1 ), C-H stretching

6 86 J. Krean Electrchem. Sc., Vl. 1, N. 1, 009 Fig. 8. FT-IR spectra recrded befre cycling and after 100 cycles: (a); uncated and (b); ml% ITOcated cathde. (850~970 cm 1 ), C O stretching (1690~1760 cm 1 ), C-O bending (1050~1300 cm 1 ) ƒ š, Yazami šw carbnates» ƒ y w(xidative decmpsitin) s e p (plycarbnates)» w q. x 19,0) 181, 1516, 11, 1136, 1100, 853, 796 cm vjƒ 1, gq 100z w z rp vj j w, ITOƒ gq z rp yƒ š, C-H stretching (850~970 cm 1 ) w vj ùkû. l, gq w ECù DMCƒ y w ROCO Li ROLi sww v x w, w v w f»w, ƒ w š w. ù ITOƒ gq w w v x ƒƒ š, j w š q w. wr, ITO gqw p w (Fig. 5), ITO w j v x l ƒ w. 5. ITO gqw z š sƒw. gq š š w y w w t w j v š, ƒw w. ITO gqw t w w wƒ š, v x w x w. w x ITOƒ gq j p p w. ù, p w ITO»» w q. y l mw w w w,. š x 1. J. Desilvestr and O. Haas, 'Metal Oxide Cathde Materials fr Electrchemical Energy Strage: A Review' J. Electrchem. Sc., 137, 5C (1990).. S. Megahed and B. Scrsati, 'Lithium-in Rechargeable Batteries' J. Pwer Surces, 51, 79 (199). 3. C. Sigala, D. Guymard, A. Vebaere, Y. Piffard, and M. Turmus, 'Psitive Electrde Materials with High Operating Vltage fr Lithium Batteries: LiCr y Mn -y (0ß yß 1)' Slid State Inics, 81, 167 (1995).. R. J. Gummw, A. de Kck, and M. M. Thackeray, 'Imprved Capacity Retentin in Rechargeable V lithium/ lithium manganese xide (spinel) cells' Slid State Inics, 69, 59 (199). 5. Y. Y. Xia, Y. H. Zhu, and M. Yshi, 'Capacity Fading n Cycling f V Li/ Cells' J. Electrchem. Sc., 1, 593 (1997). 6. J. M. Tarascn, W. R. Mckinnn, F. Cwar, T. N. Bwmer, G. Amatucci, and D. Guymard, 'Synthesis Cnditins and Oxygen Stichimetry Effects n Li Insertin int the Spinel ' J. Electrchem. Sc., 11, 11 (199). 7. D. Guymard and J. M. Tarascn, 'The carbn/li 1+x Mn system' Slid State Inics, 69, (199). 8. Y. Ga and J. R. Dahn, 'Crrelatin between the grwth f the 3.3 V Discharge Plateau and Capacity Fading in Li 1+x Mn -x Materials' Slid State Inics, 8, 33 (1996). 9. Y. Ga and J. R. Dahn, 'Synthesis and Characterizatin f Li 1+x Mn fr Li-In Battery Applicatins' J. Electrchem. Sc., 13, 100 (1996). 10. Y. Xia and M. Yshi, 'An Investigatin f Lithium In Insertin int Spinel Structure Li-Mn-O cmpunds' J. Electrchem. Sc., 13, 85 (1996).

7 w»ywz, 1«, 1 y, D. H. Jang, Y. J. Shin, and S. M. Oh, 'Disslutin f Spinel Oxides and Capacity Lsses in V Li/Li x Mn cells' J. Electrchem. Sc., 13, 0 (1996). 1. G. H. Li, H. Ikuta, and T. Uchida, 'The Spinel Phases LiM y Mn -y (M = C, Cr, Ni) as the Cathde fr Rechargeable Lithium Batteries' J. Electrchem. Sc., 13, 178 (1996). 13. S. T. Myung, S. Kmaba, and N. Kumagai, 'Enhanced Structural Stability and Cyclability f Al-Dped Spinel synthesized by the Emulsin Drying Methd' J. Electrchem. Sc., 18, A8 (001). 1. A. M. Kannan, L. Rabenberg, and A. Manthiram, 'Surface/ Chemically Mdified Cathdes fr Lithium-In Batteries' Electrchem. Slid-State Lett., 5, A167 (00). 15. M. M. Thackeray, C. S. Jhnsn, J.-S. Kim, K. C. Lauzze, J. T. Vaughey, N. Dietz, D. Abraham, S. A. Hackney, W. A. Zeltner, and M. A. Andersn, 'ZrO - and Li ZrO 3 -stabilized Spinel and Layered Electrdes fr Lithium Batteries' Electrchem. Cmmun., 5, 75 (003) 16. Y. K. Sun, K. J. Hng, and J. Prakash, 'The Effect f ZnO Cating n Electrchemical Cycling Behavir f Spinel Cathde Materials at Elevated Temperature' J. Electrchem. Sc., 150, A970 (003). 17. J. P. Ch, T. J. Kim, Y. J. Kim, and B.W. Park, 'Cmplete Blcking f Mn 3+ in Disslutin frm a Spinel Intercalatin Cmpund by C 3 Cating' Chem. Cmmun., 1, 107 (001) 18. D. Aurbach, K. Gamlsky, B. Markvsky, G. Salitra, and Y. Gfer, 'The Study f Surface Phenmena Related t Electrchemical Lithium Intercalatin int Li x MO y Hst Materials (M = Ni, Mn)' J. Electrchem. Sc., 17, 13 (000). 19. A. Duglas and F. Skg, James Hller and Timthy A. Nieman, Principles f Instrumental Analysis, 5th editin, pp. 10, Harcurt Brace Cllege Publishers, USA (1998). 0. R. Yazami, 'Surface Chemistry and Lithium Strage Capability f the Graphite-Lithium Electrde' Electrchim. Acta, 5, 87 (1999).

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