Transition metal-containing composite hydroxide and production method, non-aqueous electrolyte secondary battery, positive electrode active material and production method thereof
A composite hydroxide and cathode active material technology, applied in the direction of non-aqueous electrolyte batteries, secondary batteries, active material electrodes, etc., to achieve the effect of low cost, great industrial significance, and excellent battery characteristics
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Embodiment 1
[0292] a) Manufacture of composite hydroxide
[0293] [nucleation process]
[0294] First, in a 60L reaction tank, 14L of water was added and stirred, and the temperature in the tank was set to 40°C. At this time, nitrogen gas was circulated in the reaction tank for 30 minutes, and the reaction atmosphere was made into a non-oxidizing atmosphere with an oxygen concentration of 2% by volume or less. Next, an appropriate amount of 25% by mass of sodium hydroxide aqueous solution and 25% by mass of ammonia water was supplied to the reaction tank, the pH value was adjusted to 12.8 based on the liquid temperature of 25° C. and the ammonium ion concentration was adjusted to 10 g / L, thereby , forming an aqueous solution before the reaction.
[0295] At the same time, nickel sulfate, cobalt sulfate, manganese sulfate, and zirconium sulfate were dissolved in water, and the molar ratio of each metal element was Ni:Mn:Co:Zr=33.1:33.1:33.1:0.2, and a 2mol / L raw material aqueous solution...
Embodiment 2
[0333] In the particle growth process, after 60 minutes (relative to 25% of the total time of the particle growth process) from the start of the particle growth process, switching operation 1 was performed, and after 5 minutes (relative to 25% of the total time of the particle growth process) after switching operation 1 2.1%), then switch operation 2, and then continue the crystallization reaction for 175 minutes (72.9% relative to the total time of the particle growth process), except that, in the same manner as in Example 1, a composite hydrogen oxidation solution was obtained. materials, positive electrode active materials and secondary batteries, and evaluated. The results are shown in Tables 2 to 4.
Embodiment 3
[0335] In the particle growth process, after 60 minutes (relative to 25% of the total time of the particle growth process) from the start of the particle growth process, switching operation 1 is performed, and after 15 minutes (relative to 25% of the total time of the particle growth process) from switching operation 1 6.3%), then switch operation 2, and then continue the crystallization reaction for 165 minutes (relative to 68.8% of the total time of the particle growth process), except that, in the same manner as in Example 1, a composite hydroxide was obtained. , positive electrode active material and secondary battery, and evaluate them. The results are shown in Tables 2 to 4.
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