将钛酸四丁酯和P123(聚环氧乙烷-聚环氧丙烷-聚环氧乙烷三嵌段共聚物)超声分散于叔丁醇中,在微波辐射下加入醋酸锂溶液制备出较小粒径且形貌单一的Li4Ti5O12(LTO)前驱体,350℃空气中预烧3 h后,600℃下隔绝空气煅烧8 h得到尖晶石碳包覆LTO(LTO/C)。采用扫描电子显电镜、透射电镜和LAND CT2001A电池测试系统等对此材料进行了表征。研究发现,该材料二次团聚的粒子平均粒径约2μm,表明反应溶剂叔丁醇的"软模板"作用能够形成更小尺寸的LTO前驱体粒子,形成的二次团聚的粒子较小。微波辅助能够加快水解反应并使反应物反应更加充分,P123作为表面活性剂可减小LTO前驱体粒子尺寸并且控制二次团聚大小。烧结过程中由P123形成的碳阻隔二次团聚粒子之间晶体生长发育并改善其导电性能。电化学性能测试显示:当测试倍率在0.1C时,该LTO的首次充放电比电容量为159.7 m A·h/g(理论比容量达到170 m A·h/g),在0.2C,0.5C,1C的倍率下进行测试,放电比电容量分别为147.1,121.2,95.3 m A·h/g,并具有良好的循环性能。
In this study,tetrabutyl titanate and P123 were first dispersed in tertbutanol with the help of ultrasonic wave. Then lithium acetate solution was added into the above mixture under microwave radiation to form LTO precursor with smaller particle size and better monodispersity of the morphology. After presintering at 350 ℃ in air for 3 hours, the LTO precursor was calcined at 600 ℃ for 8 hours to obtain spinel LTO/C. This material was characterized by scanning electron microscopy (SEM),transmission electron microscopy (TEM) and LAND CT2001A battery test system. The study shows that the average size of two reunion particles of this material diameter is about 2 μm because of "soft template" confinement effect of the tertbutanol which can form smaller LTO precursor and two aggregate particles. Besides,microwave can accelerate the hydrolysis reaction and the reaction is more fully. As a surfaetant in the reaction, P123 decreases LTO precursor particle size and controls the two reunion particle size. And carbon formed from P123 in sintering process impedes the growth of crystals between two reunion particles and improves the conductive properties of the material. The electrochemical performance test shows that when the test rate is 0.1C,the first discharge specific capacity of LTO is 159.7 mA · h/g(pure capacity reached 170 mA · h/g). While when it tested in O. 2C,0.5C, 1C,the first discharge specific capacity of LTO were 147.1,121.2,95.3 mA ·h/g,and the as-prepared material has a good cycle performance.