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1 Jurnal f the Krean Ceramic Sciety Vl. 45, N., pp. 67~7, 008. Structural Stability During Charge-Discharge Cycles in Zr-dped LiCO Pwders Sen Hye Kim*, Kwang-B Shim**, Jae-Pyung Ahn***, and Chang-Sam Kim Battery Research Center, Krea Institute f Science and Technlgy, Seul 6-79, Krea *Faculty f Engineering, Kyushu University, Fukuka , Japan **Divisin f Advanced Materials Science and Engineering, Hanyang University, Seul -79, Krea ***Advanced Analysis Center, Krea Institute f Science and Technlgy, Seul 6-79, Krea (Received February 0, 008; Accepted March, 008) ƒ w Zr v LiCO ½ *Á Ÿ **Á s***á½ w w» l *j w» l **w w œw ***w w» p l (008 0 ; 008 ) ABSTRACT Zircnium-dped Li C Zr O (0 0.05) pwders as cathde materials fr lithium in batteries were synthesized using an ultrasnic spray pyrlysis methd. Cyclic vltammetry and cyclic stability tests were perfrmed, and the changes f micrstructure were bserved. The slubility limit f zircnium int Li CO was less than 5 ml%, and mnclinic Li ZrO phase was frmed abve the limit. The Zr-dping suppressed the grain grwth and increased the lattice parameters f the heagnal LiCO phase. The Zr-dping f ml% resulted in the best cyclic perfrmance in the range f.0 ~ 4. V at C rate (40 ma/g); the initial discharge capacity decreased frm 58 mah/g t 60 mah/g in the undped pwder, while frm 54 mah/g t 5 mah/g in the Zr-dped pwder f ml% after 0 cycles. The ecellent cycle stability f Zr-dped pwder was due t the lw plarizatin during chargedischarge prcesses which resulted frm the delayed cllapse f the crystal structure f the active materials with Zr-dping. Key wrds : Lithium in battery, LiCO, Zr-Dping, Cycle stability, Micrstructure. y ƒ LiCO k C-O w ñ C O w w, 4. V w Li k w y w ƒ wš j j w» w. ) š» w 4. V w j w w. ù»» wì w j» y s w. y ã š, Crrespnding authr : Chang-Sam Kim Tel : Fa : y v y w. ƒ š LiCO j» 5 ~ 0 µm. j yww j w œ. ù j w w w j» w g pƒ w w ƒ. LiCO j p w j» w, C eyw ù LiCO t gq w w ƒ y w š. -5) LiCO Zr ƒw wù j p p w š š. Zrey 6,7) w p w ƒ, LiO 6 ctahedral inter-slab ƒ ù Li y ü w v w y y ƒ w» š, XRD XANES w ƒ š w. 7) wr, j p 67

2 68 ½ Á Ÿ Á sá½ w + Li j»ƒ w Zr ƒ C ƒ Li ey š ƒ wš, Li ù Zr Lid w» w w» š wš. 6) q w w µm Zr ey LiCO w w»yw p wš p y w j p w w wš w.. Zr ƒ Li (C Zr )O (=0, 0.005,, 0.05) q w w w z z w. w w LiNO (99.95%, Kant chemical, Japan) C(NO ) 6H O (98%, Junsei, Japan), ZrO(NO ) H O(99.5, Aldrich, USA) w. p w» w yw 0% ƒw. ƒ s w yw ƒ 0.5 ml/l..67 MHz q w y w, ƒ 5l/min 70 mm ¼ 00 mm w. 400 C, 800 C w g. vl( µm, 5C, Advantic) w s w. s w z, s w r k z 600 C¾ 5C/min w š, 600 C l C/min 900 C¾ g 0 w z þw. z ƒ ó ù w w. y y w» w XRD (mdel D/ Ma-A, Rigaku, Japan) w 40 kv, 0 ma CuKa graphite mnchrmatr filter w. SEM(Mdel S-400, Hitachi, Japan) TEM(TECNAI G F0, FEI, The Netherlands) w w y»yw z w. w Zr ƒ C yƒ y NEXAFS (near edge X-ray absrptin spectrscpy) w w. w sw ƒ» KIST (80 ~ 800 ev sft -ray). Ÿ X Ÿ { duble crystal mnchrmeter Si() w. reference d w C fil rp (C K- edge = 7709 ev) ùkù vj e w w» w.»yw d g (type 0) w w w. w w y AB(acethylene black) š w PVDF(plyvinylidene fluride) [5% in NMP(-methyl--pyrrlinne)] 90:5:5 z, 5 mm j» g š NMP (-methyl--pyrrlinne) ƒw slder paste mier w ³ w w. y ~ 0 µm Ì swš, 80 C k z,» w w. z, j» punching» w 6 mm z, w œ g y. y p fil, w wetting PP(ply prpylene) w w. w EC(ethylene carbnate) : EMC(ethylmethyl carbnate) : DMC(dimethyl carbnate) = : : M LiPF 6 w š» w w. (Galvanstatic),.0~4. V 50z w., j 0.C w, j l C w. w CV.0 ~ 4.5 V¾ mv/s ww.. š Fig. Zr ƒ XRD ql, q w w w Li C Zr O 900 C 0 w. 8 (006) (0) š 66 (08) (0) vjƒ, w d ƒ Rm α- NaFeO. Li C Zr O 0 Fig.. XRD patterns f (a) Li CO, (b) Li C Zr O, (c) Li C 0.99 Zr O, and (d) Li C 0.95 Zr 0.05 O pwders annealed at 900 C fr 0 h. w wz

3 충방전 과정중 구조가 안정한 Zr이 도핑된 LiCO 분말 69 Structural Parameters f Li C Zr O Pwders R a-lattice c-lattice I /I Table X 범위에서는 이차상 피크가 발견되지 않았으나, Zr 이 5 ml% 치환된 경우에는 단사정계인 Li ZrO 피크가 보여, ml% 첨가까지는 Zr 고용이 가능하지만 그 이상 첨가되면 이차상이 나타나는 것을 알 수 있었다. I /I 비는 층상구조의 양이온혼합정도를 나타내는 척도로써, =0, 0.005,, 0.05에서 각각 5.6,.8,.0,.78로 감소하는 경향을 보여, Zr이 첨가되면 양이온들의 혼합이 증가하는 것을 알 수 있었다. Table 은 각 분말의 격자 상수를 보여주고 있다. 각 분말의 a, c축의 격자상수는 최 소자승법 프로그램에 의해 육방정계로 설정하여 구한 결 과이다. Zr이 치환된 결과를 비교해 보면 Zr의 치환량이 증가할수록 a, c축의 격자상수가 증가하고 있음을 알 수 있다. 그러나 5 ml% 첨가하여 이차상이 생성된 경우는 오히려 격자상수가 감소하였다. 이것은 Zr의 첨가량이 많 아지면 단사정계인 Li ZrO 가 생성되기 때문인 것으로 사 료되었다. 한편 치환에 의한 격자상수의 변화는 치환되는 입자사이의 이온반경 차이와 산화수의 차이에 의한 정전 기적 힘의 차이에 의해서 일어난다. 6배위를 하고 있을 때 Zr 의 이온반경은 0.7 Å으로 C (0.65 Å), C (0.55 Å)보다 크기 때문에 Zr이 C 자리에 치환되면 격자상수 가 증가할 수 있다. 한편 Li 이온반경은 0.76 Å로 Zr 의 이온반경과 비슷하나, Zr이 Li 자리에 치환되었을 때 인 접한 Zr 와 C 의 정전기적 반발력이 Li 와 C 의 반 발력보다 크기 때문에 격자상수가 증가할 수 있다. 어느 경우이거나 격자상수가 증가한 것은 Zr이 치환되었다는 것을 나타내고 있다. 그리고 Zr의 치환양은 초음파분무열 분해법으로 합성하였을 경우 이차상이 나타나지 않은 5 ml% 미만으로, 이것은 졸겔법으로 Zr을 첨가한 경우와 유사한 결과이었다. Fig. 는 900 C에서 0시간 열처리한 분말의 형상을 관 찰한 사진이다. Zr을 첨가하지 않은 분말은 대부분의 입 자크기가 µm 이상이며, 최대 4 µm 정도의 입자도 다수 관찰되었다. Zr 치환량이 증가함에 따라서 입자크기는 작 아졌는데 ml% 첨가되었을 때의 평균입경이 ~ µm로 첨가하지 않았을 때보다 현격하게 작아졌으나, 그 이상 첨가된 경우에는 더 이상 작아지지 않았다. Fig. 은 Zr이 첨가된 분말과 C의 산화정도를 비교하 기 위해서 사용한 CO와 C O 분말의 C L-edge의 NEXAFS 스펙트럼이다. 산화수가 높을수록 높은 에너지 영역에서 피크가 나타나기 때문에, 대부분의 C 산화수 Fig.. SEM images f Li (C Zr )O ( = 0, 0.005,, 0.05) annealed at 900 C fr 0 h. 8) ) 4 + Fig.. C L-edge NEXAFS spectra f Li (C Zr )O, C O and CO. 4 가 가로 예상되는 Li CO 분말의 피크가 가장 높은 에너지 영역이 있으며, Zr이 첨가되면서 피크가 낮은 에 너지 쪽으로 이동하고 있어, Zr이 첨가되면서 C의 산화 수가 감소하는 것을 알 수 있다. 그러나 ml%와 5 ml% 치환한 것의 피크 위치는 같았으며, 이 결과는 XRD 에서 Li ZrO 이차상이 나타나지 않는 5 ml% 미만이 Zr 의 고용한계라는 결과와 일치하는 결과이다. Fig. 4는.0~4.5 V까지 mv/s의 주사속도에서 CV 를 측정한 것이다. SEI (slid electrlyte interface)가 생성 되기 전의 첫 싸이클과 SEI가 생성된 후의 두 번째 싸이 클 사이에서는 산화전위와 환원전위의 변화가 Zr의 첨가 에 상관없이 발생하였다. 그러나 SEI가 생성된 번째 싸 이클 이후에 Zr이 치환되지 않은 활물질에서는 싸이클이 진행됨에 따라서 산화전위는 높아지고, 환원전위는 낮아지 는 분극현상이 현저하게 일어나고 있었다. 이에 대하여, Zr 이 ml% 첨가된 활물질에서는 산화환원 전위에 변화가 제 45 권 제 호(008)

4 김선혜 심광보 안재평 김창삼 70 Fig. 5. Fig. 4. Discharge capacity as a functin f cycle numbers fr cells perated at C(40 mah/g) in vltage ranges.0 4. V. Cyclic vltammgrams f (a) Li CO and (b) Li C Zr O in a vltage range f.0 ~ 4.5 V at a scan rate f mv/s 없어 활물질에 분극이 일어나지 않았음을 알 수 있다. 분 극이 커지는 것은 Li 이온이 활물질 내부로 삽입/탈리를 반복함에 따라서 활물질에 비가역적인 구조 변화가 일어 난 것을 의미한다. Zr이 ml% 첨가된 활물질에서 산화 환원전위에 변화가 없다는 것은 충방전시에 구조가 가역 적으로 변화하고 있다는 것으로, 이러한 결과에서 Zr이 ml% 첨가된 활물질은 우수한 싸이클 특성을 나타낼 것 으로 예상되었다. Fig. 5는 Zr이 첨가되지 않은 것과 0.5 ml%, ml% 첨가된 활물질로 조립한 셀의 싸이클 특성 결과이다. 첫 싸이클의 용량은 Zr을 치환하지 않는 셀에서 가장 높은 58 mah/g 이었으며, Zr을 치환함에 따라서 감소하여 ml% 치환되었을 때는 5 mah/g이 되었다. 그러나 Zr을 치환하지 않은 셀은 0 싸이클까지 거의 직선적으로 방 전용량이 급격히 감소하여 0 싸이클 후에는 60 mah/g 한국세라믹학회지 Fig. 6. TEM images f LiCO pwders (a) befre cycle test and (b) after 50 cycles, and Li C Zr O pwders (c) befre cycle test and (d) after 50 cycles 이하가 되었다. 반면 Zr이 치환된 것은 0 싸이클까지 거 의 방전용량이 감소하지 않았으며, 특히 ml% 치환된 셀은 0 싸이클 후에도 40 mah/g 이상의 방전용량을 나 타내어 예상되었던 것과 같이 우수한 싸이클 특성을 나 타내었다.

5 Fig. 6 Zr ƒ Zr ml% ƒ j z y» w TEM w. t Zr ƒw ù ƒw ñ, Zr ƒw t ƒ. w ü ü w ùkù. wr, 50z j z Zr eyw eyw j ƒ. eyw ù ü w ƒwš, ƒ wù w w t e. Zr ƒ, ü w ƒw t ñ k wš. Wang LiCO j z TEM w j z ü w ƒwš ü ³ w w. 9), Zr ƒ w j p w wùƒ, Zr ey ù ü w w w ƒ». ù Zr w w w w y w, w Dahn ZrO y t gqw, Zr t» wš ü 0) w SEI g y w j p w g ƒ» y w» w HRTEM, EELS w w ww v ƒ. 4. Zr ƒ Li C - Zr O (0 0.05) q w w w w. w Zr š w 5ml%, š w ü Zr ƒ w j š, yw ƒ ƒw. š w Li ZrO ƒ. Zr ƒ w»yw p j w, w y ù j, j p j w. w»yw p ƒ w Zr v LiCO 7 w Zr ey y ƒ w wù y w. Acknwledgment w w» p w»» š y w. REFERENCES. S. T. Myung, N. Kumagai, S. Kmaba, and H. T. Chung, Effects f Al Dping n The Micrstructure f LiCO Cathde Materials, Slid State Inics, 9 [-] (00).. Y. J. Kim, T. J. Kim, J. W. Shin, B. W. Park, and J. P. Ch, The Effect f Al O Cating n the Cycle Life Perfrmance in Thin-film LiCO Cathdes, J. Electrchem. Sc., 49 [0] A7-4 (00).. Z. Wang, C. Wu, L.Liu, F. Wu, L. Chen, and X. Huang, Electrchemical Evaluatin and Structural Characterizatin f Cmmercial LiCO Surfaces Mdified with MgO fr Lithium-In Batteries, J. Electrchem. Sc., 49 [4] A466-7 (00). 4. I. Saadune and C. Delmas, On The LiNi 0.8 C 0. O System, J. Slid State Chem., 6 [] 8-5 (998). 5. S. Oh, J. K. Lee, D. Byun, W. I. Ch, and B. W. Ch, Effect f Al O Cating n Electrchemical Perfrmance f LiCO as Cathde Materials fr Secndary Lithium Batteries, J. Pwer Surces, [-] (004). 6. H. S. Kim, T. K. K, B. K. Na, W. I. Ch, and B. W. Ch, Electrchemical Prperties f LiM C O [M = Mg, Zr] Prepared by Sl-Gel Prcess, J. Pwer Surces, 8 [-] -9 (004). 7. S. H. Kim and C. S. Kim, Imprving The Rate Perfrmance f LiCO by Zr Dping, J. Electrceram., accepted. 8. K. Kang and G. Ceder, Factrs That Affect Li Mbility in Layered Lithium Transitin Metal Oides, Phys. Rev. B, 74 [9] (006). 9. H. Wang, Y. I. Jang, B. Huang, D. R. Sadway, and Y. M. Chiang, Electrn Micrscpic Characterizatin f Electrchemically Cycled LiCO and Li(Al,C)O Battery Cathdes, J. Pwer Surces, (999). 0. Z. Chen and J. R. Dahn, Methds t Obtain Ecellent Capacity Retentin in LiCO Cycled t 4.5 V, Electrchimi. Acta, 49 [7] (004). 45«y(008)

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