Abstract LiNi 0.8 Co 0.1 Mn 0.1 O 2 cathode was synthesized using transition metal acetates under different synthesis conditions. Simultaneous thermogravimetric–differential scanning calorimetry–derivative thermogravimetric analysis was applied to investigating the mixture of transition metal acetates. X-ray powder diffraction and charge–discharge test were adopted to characterize the as-prepared LiNi 0.8 Co 0.1 Mn 0.1 O 2 . The mixture of transition metal acetates undergoes dehydration and decomposition during heating. All the examined LiNi 0.8 Co 0.1 Mn 0.1 O 2 samples have a layered structure with space group. LiNi 0.8 Co 0.1 Mn 0.1 O 2 samples prepared with different lithium sources under different synthesis conditions exhibit very different charge–discharge performances. The sample synthesized via the procedure of sintering at 800 °C after heating lithium carbonate and transition metal acetates at 550 °C achieves a highest capacity of 200.8 mA·h/g and an average capacity of 188.1 mA·h/g in the first 20 cycles at 0.2 C .