(1. 中南大學(xué) 冶金科學(xué)與工程學(xué)院，長(zhǎng)沙 410083；2. 長(zhǎng)沙礦冶研究院，長(zhǎng)沙 410012)
摘 要: 以TiCl4水溶液和LiOH·H2O為原料，采用原位水解與后續(xù)熱處理相結(jié)合的方法制備尖晶石型鋰離子電池用負(fù)極材料Li4Ti5O12。結(jié)果表明：從TiCl4水溶液原位水解合成Li4Ti5O12經(jīng)歷由TiCl4→TiO2→Li2TiO3→Li4Ti5O12 3個(gè)階段的原位相轉(zhuǎn)變過(guò)程；TiCl4水溶液的濃度及穩(wěn)定性對(duì)合成Li4Ti5O12的結(jié)構(gòu)有較大的影響；隨著TiCl4濃度的增加，合成純Li4Ti5O12所需的水解時(shí)間延長(zhǎng)；以0.5 mol/L TiCl4水溶液水解1 h、以添加1.0 mol/L LiCl的0.5 mol/L TiCl4水溶液水解3 h、以1.0 mol/L與1.5 mol/L TiCl4水溶液水解5 h均可獲得純Li4Ti5O12；由低濃度TiCl4水溶液合成的Li4Ti5O12循環(huán)性能優(yōu)良。
關(guān)鍵字: 鋰離子電池；負(fù)極材料；尖晶石Li4Ti5O12；原位水解
lithium ion batteries via in-situ hydrolysis
（1. School of Metallurgical Science and Engineering, Central South University, Changsha 410083, China;
2. Changsha Research Institute of Mining and Metallurgy, Changsha 410012, China）
Abstract:Spinel Li4Ti5O12 as an anode material for lithium ion batteries was synthesized via in-situ hydrolysis followed by heat treatment using aqueous TiCl4 solution and LiOH·H2O as the raw materials. The results show that the synthesis of Li4Ti5O12 from aqueous TiCl4 solution by in-situ hydrolysis consists of three-step in-situ phase transformation, that is TiCl4→TiO2→Li2TiO3→Li4Ti5O12. The concentration and stability of aqueous TiCl4 solution have significant effects on the synthesis of Li4Ti5O12. With increasing TiCl4 concentration, the hydrolysis time of TiCl4 for the formation of Li4Ti5O12 increases. The optimal hydrolysis time for the synthesis of pure Li4Ti5O12 from TiCl4 solutions with different Ti(Ⅳ) concentrations is found to be 1 h for 0.5 mol/L TiCl4, 3 h for 0.5 mol/L TiCl4 with addition of 1.0 mol/L LiCl and 5 h for both 1.0 mol/L and 1.5 mol/L TiCl4. The products prepared from lower Ti(Ⅳ) concentration solutions show excellent cycling performance.
Key words: lithium ion batteries; anode material; spinel Li4Ti5O12; in-situ hydrolysis
