采用固相合成法制备了具有良好层状结构的LiCo1/3Ni1/3Mn1/3O2.通过化学方法对其进行去锂处理,制备了LixCo1/3Ni1/3Mn1/3O2(0.5≤≤1)系列样品,并利用XRD、TEM以及HR-TEM等方法对其微观结构进行了系统表征.计算与实验结果表明.当0.778≤x＜1时LixCo1/3Ni1/3Mn1/3O2的结构依旧保持O3结构,而当0.5≤x＜0.778时其结构由初始的六方结构转变为单斜结构,同时电子衍射花样模拟及高分辨像模拟证明其对称性由R3m转变为P2/m.锂离子与去锂后形成的空位的有序排列是其对称性发生转变的主要原因.DSC/TG实验表明,LixCo1/3Ni1/3Mn1/3O2的热稳定性随去锂程度的不断加深而减弱;当加热至300～400℃时发生了由单斜结构向尖晶石结构转变的放热反应.
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