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1 «22 «5 Æ Ç Vol. 22, No À 9 ³ Journal of Inorganic Materials Sep., 2007 Ç : X(2007) » LiNi 0.5 x Co 2x Mn 0.5 x O 2 Æ º ÔÒ Ó Ð Ó Ñ ( Ï ) Æ Ã Ç ÊÉ É Ni 0.5 xco 2xMn 0.5 xco 3(x=0.075, 0.1, 1/6) ß Ñ Æ LiNi 0.5 xco 2xMn 0.5 xo 2(x=0.075, 0.1, 1/6), LiNi 0.5 xco 2xMn 0.5 xo 2 À Ó Æ Ç À ¾ SEM ¹ LiNi 0.5 xco 2xMn 0.5 xo 2 Â Ð Õ Í É Á Ï Ð Õ Ø XRD ¹ LiNi 0.5 xco 2xMn 0.5 xo 2 Í» Ì Æ Ç À ²» LiNi 0.5 xco 2xMn 0.5 xo 2 É Æ ÓË À 0.2C ³ V ÆκРLiNi 0.425Co 0.15Mn 0.425O 2 Ƴ 145mAh g 1 LiNi 0.4Co 0.2Mn 0.4O 2 150mAh g 1 LiNi 1/3 Co 1/3 Mn 1/3 O 2 158mAh g 1, Ë 50 LiNi 0.425Co 0.15Mn 0.425O 2 Ó LiNi 0.4Co 0.2Mn 0.4O 2 ¾³¹ 3% LiNi 1/3 Co 1/3 Mn 1/3 O 2 Æ ¾ Ñ ¹ É Ñž ÑÆ LiNi 0.5 xco 2xMn 0.5 xo 2 Ë ² TM912 µ A Synthesis and Electrochemical Performance of Spherical LiNi 0.5 x Co 2x Mn 0.5 x O 2 ZHU Yong-Jun, LI Xin-Hai, WANG Zhi-Xing, YANG Zhi, HU Qi-Yang (School of Metallurgical Science and Engineering, Central South University, Changsha , China) Abstract: Spherical LiNi 0.5 x Co 2x Mn 0.5 x O 2 (x=0.075, 0.1, 1/6) powders were synthesized from the co-precipitated carbonate precursor, Ni 0.5 x Co 2x Mn 0.5 x CO 3 (x=0.075, 0.1, 1/6). The effects of the Co content on the physics and electrochemical performance of LiNi 0.5 x Co 2x Mn 0.5 x O 2 were investigated. The SEM images of LiNi 0.5 x Co 2x Mn 0.5 x O 2 show that the spherical material consists of many primary particles, which sizes increase with the content of Co increasement. The results of X-ray powder diffraction show that all LiNi 0.5 x Co 2x Mn 0.5 x O 2 are pure phase materials with layered structures. The electrochemical tests indicate that the discharge capacities of LiNi 0.5 x Co 2x Mn 0.5 x O 2 increase and the cycle performances become better with the content of Co increasing. Under the charge/discharge conditions of 0.2C rate and voltage range of V, the discharge properties of spherical LiNi Co 0.15 Mn O 2, LiNi 0.4 Co 0.2 Mn 0.4 O 2 and LiNi 1/3 Co 1/3 Mn 1/3 O 2 are 145,150 and 158 mah g 1, respectively. The discharge capacity fadings for LiNi Co 0.15 Mn O 2 and LiNi 0.4 Co 0.2 Mn 0.4 O 2 are less than 3%, however, there is no fade for that of LiNi 1/3 Co 1/3 Mn 1/3 O 2 after 50 cycles. The results of AC impedance show that the impedance decreases with the content of Co increasing. Key words: Li-ion battery; cathode material; spherical; LiNi 0.5 x Co 2x Mn 0.5 x O 2 ¾¹ , ¾¹ ÎÈ (1982 ), ½ ²Å ³ ½ Å csuzyj@163.com

2 874 Æ Ç 22 1 ÄÀ Ø LiCoO 2 Ò ¼ ØÆ ²Ð Á ÛÚ À Þ Ú ÀÇ «Ò ±Ô Á«Â ««LiCoO 2 ±À Á Ø Ý «Ò ± Á Ò Î Ò Ù [1]. LiCoO 2 ¼ÒÀÎ LiNiO 2 Ø Ôº ¼ «ºÛ Û É± LiNiO [2] 2, Ô LiNiO 2 º Jahn-Teller ÇÌÅÁ [3]. ¹Ì ÀÎ LiMn 2 O 4 À Á ½ LiMnO 2 «É Å Ï ÌÝ Mn 3+ Å Û ³ À [1,4]. Ýß Â «Âº º ÞÊ À ÌÅ Á Å Û Â Đ «Ohzuku Ð À ¼ ¹ Ã Ø α-nafeo 2 À Î LiNi 0.5 Mn 0.5 O 2 º V Ú 150mAh g 1 «De-Cheng Li Æ ½ Ê LiNi Mn Co 0.15 O 2 º V, 0.5C Ú º 150mAh g 1, º Æ À Ì Å Á [5]. LiNi 0.5 Mn 0.5 O 2 Đ Ç Ô µ Ú Ò ÌÅÁ [5,6]. Ohzuku  Рº Õ Õ Ø Ø LiNi 1/3 Mn 1/3 Co 1/3 O 2 º V, Ø 0.125C 225mAh g 1. º 20C º 150mAh g 1 Ø Ò Å Æ Ì Å Á [7]. º º Li + Ù / LiMn 1/3 Co 1/3 Ni 1/3 O 2 À Î LiMnO 2 LiNiO 2 Ô LiCoO 2 ¼ «±Æ LiCoO 2 LiNiO 2 Ô LiNi 0.5 Co 0.5 O 2 Þ cm 2 s cm 2 s cm 2 s 1, Ò Å Co Ú Ø À Li + Þ Â [2,8]. Õ LiNi 0.5 x Co 2x Mn 0.5 x O 2 ¼  ºÔĐ Å Ê Ô ± Ò ÉÁ ÌÅÁ ÅÆ Ô Ê Đ Âº Ò Ê Ò Ý ß Þ Đ LiNi 0.5 x Co 2x Mn 0.5 x O 2» µæá ØÇ Ý Ï Ø Â Đ º» Ô ÐÛĐÄ «Ø Á µæá ÅÆ» À Øʼ À Ò [2,9 11], ± Ø Ò Đ» À Ø Â Đ º ¼ Á Ô É Á É «ËÊ ½ Ê ÒĐ Ø Ni 0.5 x Co 2x Mn 0.5 x CO 3 (x= /6), Đ ¼ Ø À» Ø LiNi 0.5 x Co 2x Mn 0.5 x O 2 (x= /6). 2 Á 2.1 ¼ Ni 0.5 x Co 2x Mn 0.5 x CO 3 Ê» NiSO 4 6H 2 O CoSO 4 6H 2 O MnSO 4 4H 2 O ± 0.425:0.150:0.425, 0.4:0.2:0.4 Ô 1/3:1/3:1/3 Å Õ Ã 2mol L 1 Æ 2mol L 1 Na 2 CO 3 ¹ ± µ  500r min 1 ¹ Ò µ Ñ º 50 C ¹ Ñ» Ø Ni Co 0.15 Mn CO 3 Ni 0.4 Co 0.2 Mn 0.4 CO 3 Ô Ni 1/3 Co 1/3 Mn 1/3 CO 3, Ï Â Ò Å º 80 C Þ Ni Co Mn Ø Ä «2.2 ¼ LiNi 0.5 x Co 2x Mn 0.5 x O 2 Å Ø Ni 0.5 x Co 2x Mn 0.5 x CO 3 º Ñ Ï Li Õ Æ ± 1:1 Å Li 2 CO 3, Ø µđº 900 C Ý 12h, Ê LiNi 0.5 x Co 2x Mn 0.5 x O XRDÅ SEM É Ï É XRD À Î º Ó D/max-A X ¹ Ó ( ± É). JEOL È À JSM-5600LV ¾ Ï Ë «2.4  «ÍÌ Ê Á Í Õ Ù Ç Õ (PVDF) À Í 90: 6: 4 Ø Ø N- ß ÛÑ (NMP) Æ Ê º º 140 C ½ĐÊ Ø Ø ( Â) 1.0mol L 1 LiPF 6 /EC+DMC( 1:1) Ý Â Celgarg 2300  Š½ «Ó ( Ð ) É ÌÅÁ «Ý / ÝϽ É Ï» V.

3 5 LiNi 0.5 xco 2xMn 0.5 xo 2 Æ ÇÀ 875 CH1660 É Æ Ý ( Ç Ó È À) É Ø Ò Ê» 0.01Hz 100kHz, ±½ Ï Ð Æ 5mV. º V Â»Ø 0.2C Ñ ÄÌÅĐÉ ØÒ 4.3V ØÒ Á«3 3.1 ¼ Ni 0.5 x Co 2x Mn 0.5 x CO 3 Ü Ê À Ì É Ë Ê Ê Ni 0.5 x Co 2x Mn 0.5 x CO 3 Ë Ü Û Á Ô Á «Ö 1 Ê Ni 0.5 x Co 2x Mn 0.5 x CO 3 SEM Ö «Ú Ø Ni 0.5 x Co 2x Mn 0.5 x CO3 Ø À Ö Å Ú º 15µm Ú Å º ½ ³ Æ Ç»» 2.0g cm 3, Ø Ú Ø Ø À» Ò LiNi 0.5 x Co 2x Mn 0.5 x O LiNi 0.5 x Co 2x Mn 0.5 x O 2 É Ö 2 ϼ LiNi 0.5 x Co 2x Mn 0.5 x O 2 SEM Ö ÚØ Ø Ni 0.5 x Co 2x Mn 0.5 x CO 3 Ø LiNi 0.5 x Co 2x Mn 0.5 x O 2 Ø Æ Ø ÖÅ Ä ÑÐÖÅÙ «À Ú SEM Ö Ú Æ(a) Ö Â ÑÐÖÅ (c) Ö Â ÑÐ ÖÅ ÓÚ (e) Ö Â ÑÐÖÅ Ý ³Æ ¾ Ì «SEM Ö º 2x 0.15((b) Ö) Ô 1/3((f) Ö) Ø Öź½ Ñ ÐÖÅ µ (b) Ö Ø ÖÅ ÑÐÖÅ (f) ÖØ ÖÅ ÑÐÖż ÓÚ 2x 0.2 (d) Ö Ø Öź½ ÑÐÖÅ ÀÌÝ Ø ÑÐÖÅ «Ú Đ µ LiNi 0.5 x Co 2x Mn 0.5 x O 2 Ø Ô¹Ñ ÐÖÅ ³Æ Đ ²À Ì ²Ý «Î» Ú 2.2g cm 3, ÊĐÄ» «Ö 3 LiNi 0.5 x Co 2x Mn 0.5 x O 2 XRD Ö «Ö 3 ϼ Ý I 003 /I 104 Ú 1.2, (I I 012 )/I 101 º Ø LiNi 1/3 Co 1/3 Mn 1/3 O 2 Ý ÀΫÞÒÖ ¹ÚØ ßĐ À (101) (006) (102) (108) (110) ² Ý Ú À ¼ Ò Ø LiNi 1/3 Co 1/3 Mn 1/3 O 2 Đ Ì ÀÎ Â Ä º Ä Â º Ø ¼ LiNi 0.5 x Co 2x Mn 0.5 x O 2 Ø Ô«3.3 Ö 4 0.2C LiNi 0.5 x Co 2x Mn 0.5 x O 2 º V ݹ«Ö 4 º º LiNi 0.5 x - Co 2x Mn 0.5 x O 2 Ê Đ µ ÚÆ LiNi Co 0.15 Mn O 2 145mAh g 1, LiNi 0.4 Co 0.2 Mn 0.4 O 2 150mAh g 1, LiNi 1/3 Co 1/3 Mn 1/3 O 2 158mAh g 1. Ö 5 LiNi 0.5 x Co 2x Mn 0.5 x O 2 º 0.2C Ì Å Ý ¹«Ò Ö Ú Ø Ì Å 50 Ð Đ LiNi Co 0.15 Mn O 2 Ô LiNi 0.4 Co 0.2 Mn 0.4 O 2 º 3% Ø LiNi 1/3 Co 1/3 Mn 1/3 O 2 «º LiNi 0.5 x Co 2x Mn 0.5 x O 2 ÅÆ ÌÅÁ Ò Ê Đ µ ÌÅÁ À µ Co ÂĐ Æ Á Ni Ô Mn µ À Ì [12], À Î Ý Ò º Ù «Ú Co Õº¹ Ni Å Ã Ð Ç Ni 2+ Å Á Ô¹ Ni 2+ Ni 3+, Ì ÀÎ Ôº Õº Jahn-Teller ºØ +4 Õº ÌÁ Õ 1 Ni 0.5 xco 2xMn 0.5 xco 3 SEM È Fig. 1 SEM photos of the spherical Ni 0.5 xco 2xMn 0.5 xco 3 1: Ni Co 0.15 Mn CO 3 ; 2: Ni 0.4 Co 0.2 Mn 0.4 CO 3 ; 3: Ni 1/3 Co 1/3 Mn 1/3 CO 3

4 876 Æ Ç 22 Õ 2 LiNi 0.5 xco 2xMn 0.5 xo 2(x=0.075,0.1, 1/6) SEM È Fig. 2 SEM photos of LiNi 1/3 Co 1/3 Mn 1/3 O 2(x=0.075,0.1, 1/6) (a),(b): LiNi Co 0.15 Mn O 2 ; (c),(d): Li Ni 0.4 Co 0.2 Mn 0.4 O 2 ; (e),(f): LiNi 1/3 Co 1/3 Mn 1/3 O 2 Õ 3 LiNi 0.5 xco 2xMn 0.5 xo 2 XRD Õ Fig. 3 XRD patterns of LiNi 0.5 xco 2xMn 0.5 xo 2 a: LiNi Co 0.15 Mn O 2 ; b: LiNi 0.4 Co 0.2 Mn 0.4 O 2 ; c: LiNi 1/3 Co 1/3 Mn 1/3 O 2 Õ 4 LiNi 0.5 xco 2xMn 0.5 xo 2 ¹ V, 0.2C ÆÜ Fig. 4 Charge-discharge curves of LiNi 0.5 xco 2x- Mn 0.5 xo 2 at 0.2C, in the range of 2.7V to 4.3V

5 5 LiNi 0.5 xco 2xMn 0.5 xo 2 Æ ÇÀ 877 Õ 5 LiNi 0.5 xco 2xMn 0.5 xo 2 ¹ V, 0.2C ÆË À Ü Fig. 5 Cycle ability curves of LiNi 0.5 xco 2xMn 0.5 xo 2 at 0.2C, in the range of 2.7V to 4.3V Ä Î ½ Á Ñ ÙÈ ÁÒ ĐÐ Ä ÖÐ Ì Æ À Æ [13]. Ô 6 ¾ ÖÐÔ ÜĐ¾ ÖÐÔ «ÉÚ Ã Nyquist ÉÚ Ì 45 ÌÏ ¾ Ñ Ò Î ÖÐÒ Đ ¾ĐÐ º Î Ý Đ Warburg ÖÐ È Ð ³ Öн Ø Ð ³ Î Ñ Ò Ð 4.3V Ð Ö Ð Î ³ Ã Ò É Ú É Ú ¾«Đ Ð ¼ Î Ò ÖÒ Đ º Đ Ð / Á Ë Ã ¼ ¼Î Î É Ú ¾«Ñ ÒÖÐÒ Ñ Ò Đ [13 15], º ³ ± Æ Ö Ð Ñ Ö Ð Ô Ø Ö ÉÚ ÒÎÉÚ Ú È Ð ³ ĐÐ ¼ Ï ¼ÖÐÒ Ñ ÒÖÐ ½ Ö LiNi 0.5 x Co 2x Mn 0.5 x O 2 ÖÐÈ Î Ð ³ ½ Ð ¾ Î Ð ½ Ni 2+ È Đ Đ Ð Ä Ñ Ô 3 LiNi 0.5 x Co 2x Mn 0.5 x O 2 XRD ØÖ È Ð ³ (101) (006) (102) (108) Ò (110) ±ÜĐ ĐРı È Ni 2+ ÒÈ Á Li + ± Đ Ð Ä Æ Å Æ Đ Ð Ø Í Ö Đ Ð º Ò ¼ Î Ò Öº ½ Õ 6 LiNi 0.5 xco 2xMn 0.5 xo 2 ÑÕ Fig. 6 AC impedance of LiNi 0.5 xco 2xMn 0.5 xo 2 (a) Before charged; (b) At 4.3V Ceder µ Å Đ º LiNiO 2 ß LiNi 0.5 Mn 0.5 O 2 Ø ¾ «Ì Î Ä Ni Mn Á º º Ü Đ Ë Í [12] LiNi 0.5 x Co 2x Mn 0.5 x O 2 Û XPS Co Đ Ni, Mn, O Ö Co Ó Ð Ì µ È Ð ÆĐ O, Mn Ò Ni ½ Ë Î µ ĐÐ Î Ø Ô 4 LiNi 0.5 x Co 2x Mn 0.5 x O 2 0.2C ² V ¾ Û ÍÌ È Co ³ LiNi 0.5 x Co 2x Mn 0.5 x O 2 Î Đ Ð ÌÎ Ø ² ÑÑ Ä Đ Ð Ò Å ³ Ú Ð ³ Ö Ð ¾ Ñ Ò Ö Ð Ä È Ð ³ ½ 4 ÉÈ µè Ö Þ Ni 0.5 x Co 2x Mn 0.5 x CO 3 (x=0.075, 0.1, 1/6), Ö Þ ÖÏ Æ Ì º Ö LiNi 0.5 x Co 2x Mn 0.5 x O 2 (x=0.075,

6 878 Æ Ç ,1/6) Ö LiNi 0.5 x Co 2x Mn 0.5 x O 2 Æ Æ È Ð ³ È ³ Ê ± V, 0.2C ² È ¾ LiNi Co 0.15 Mn O 2 Đ 146mAh g 1, LiNi 0.4 Co 0.2 Mn 0.4 O 2 Đ 150mAh g 1,LiNi 1/3 Co 1/3 Mn 1/3 O 2 Đ 158mAh g 1 ; Ê 50 Ð LiNi Co 0.15 Mn O 2 Ò LiNi Co 0.2 Mn 0.4 O 2 ½² 3% Ö LiNi 1/3 - Co 1/3 Mn 1/3 O 2 Ê 50 Ð ½ ÖÐ È Ð ³ ÖÐ ½ LiNi Co 0.15 Mn O 2 Ò LiNi 0.4 Co 0.2 Mn 0.4 O 2 Ç Æ ² LiNi 1/3 Co 1/3 Mn 1/3 O 2 Ý «ÎÐ ±ÀÏ º Ô ÖÓ± Ð LiNi 0.5 x Co 2x Mn 0.5 x O 2 Ð Ò Ï Æ ÜÞ ± [1] Í Ñ (YE Shang-Yun, et al). Å (Chinese Journal of Rare Metals). 2005, 29: [2] «Ù (TANG Ai-Dong, et al). ÈÈ (Acta Chimica Sinica), 2005, 63(13): [3] Ä (CHANG Zhao-Rong, et al). Ã È (Journal of the Chinese Ceramic Society). 2006, 34 (3): [4] à (ZHONG Hui, et al). È È (Acta Chimica Sinica), 2004, 62(12): [5] LI De-Cheng, Hideyuki N, Yoshio M. Electrochimica Acta. 2004, 50: [6] Cho T H, Park S M. Journal of Power Sources. 2005, 142 (1 2): [7] Yabuuchi N, Ohzuku T. Journal of Power Sources, 2005, 146: [8] ß (TANG Hong-Wei). ÙȾ½È Å [9] HE Xiang-Ming, LI Jian-Jun, CAI Yan, et al. Materials Chemistry and Physics, 2006, 95: [10] Å (YING Jie-Rong, et al). È (Journal of Inorganic Materials). 2006, 21 (2): [11] Õ ÏÞ (HE Xiang-Ming, et al). Å È (The Chinese Journal of Nonferrous Metals). 2005, 15 (9): [12] Ì Î (SUN Yu-cheng). ξ½È Å [13] (ZHAO Yu-juan). Í ÙȾ½È Å [14] «Ü ˲ (HUANG You-Yuan, et al). ÈÈ (Acta Phys.-Chim.Sin.), 2005, 21 (7): [15] Ô (DU Ke). È ß Ó Î ¾½È Å 2003.

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