Spinel Li1+xMyMn2-x-yO4, preparation method thereof and lithium-ion secondary battery
A xmymn2-x-yo4, spinel technology, applied in the field of doping spinel lithium manganate, can solve the problems of irregular lithium manganate morphology, reduced material cycle performance, low material specific capacity, etc. Excellent cycle performance, high temperature cycle performance and high specific capacity
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[0037] The present invention also provides the above spinel Li 1+x M y Mn 2-x-y O 4 The preparation method includes
[0038] (1) Mixing: Mix lithium-containing compound, manganese powder and / or manganese-containing compound, and compound containing doping elements according to the chemical dose ratio, add solvent and stir evenly, transfer to ball mill in a ball mill tank, and dry to remove solvent. Mixed raw materials;
[0039] (2) High-temperature sintering of the mixed raw materials obtained in step (1) in an atmosphere containing oxygen;
[0040] (3) The Li obtained in step (2) 1+x M y Mn 2-x-y O 4 The precursor is annealed and sintered in an oxygen-containing atmosphere; it is cooled to obtain Li 1+x M y Mn 2-x-y O 4 . The preparation method of the invention is simple, low in cost and easy to realize. The prepared spinel structure lithium manganate has a wide range of applications, and the performance of the product using the lithium manganate of the invention is greatly improv...
Example Embodiment
[0054] Example 1
[0055] (1) Preparation of cathode material
[0056] Add 340g lithium carbonate (battery grade), 1400g electrolytic manganese dioxide, 70.22g cobalt nitrate (cobalt content 21%), 95.32g nonahydrate aluminum nitrate (battery grade), and 825g deionized water into a 5L mixing tank and stir After 1.5h, transfer to a 5L ball milling tank, control the ball-to-material ratio to 1:1, ball mill on a planetary ball mill at a speed of 150 revolutions / min for 2 hours, and then ball mill the material on a rake vacuum dryer (self-made, Negative pressure 0.05Mpa) Take it out after drying at 150°C for 4h. The dried material is heated in the muffle furnace at a rate of 5°C / min to 650°C, constant temperature for 6 hours, then at a rate of 3°C / min to 900°C, constant temperature for 12 hours, and then at a rate of 5°C / min The temperature was lowered to 700°C, kept at a constant temperature for 8 hours, then at a rate of 5°C / min to 500°C, kept at a constant temperature for 6 hours, ...
Example Embodiment
[0069] Example 2
[0070] The synthesis method and battery manufacturing method are the same as in Example 1, except that the raw material in the preparation of the positive electrode material contains 10.0 g of anhydrous sodium carbonate (analytical pure) and 5.2 g of magnesium nitrate hexahydrate (analytical pure).
[0071] Measure the I of the material according to the same method as in Example 1. 400 / I 311 ; 111,311,400 peak crystal plane diffraction peak half-width B value, I 311 / I 111 , I 400 / I 111 The data is shown in Table 1; the primary particle diameter is shown in Table 1.
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