A kind of preparation method of nanometerization olivine type lithium-ion battery cathode material
A lithium-ion battery, olivine-type technology, used in battery electrodes, chemical instruments and methods, circuits, etc., can solve problems such as low electronic conductivity, and achieve high ionic and electronic conductivity, excellent low-temperature performance, and high capacity. Effect
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[0033] In the preparation method of the above-mentioned nano-sized olivine-type positive electrode material, the antioxidant in step (2) is aniline, ascorbic acid, citric acid, phenol, diphenol, tocopherol, butylated hydroxytoluene, ascorbic acid sodium salt, calcium One or more of salt.
[0034] In the above-mentioned preparation method of the nano-sized olivine-type positive electrode material, except for lithium iron phosphate and lithium iron silicate, other materials may not need to pass through protective gas and add antioxidant in step (2).
[0035] In the above-mentioned preparation method of nano-sized olivine-type positive electrode materials, in addition to synthesizing lithium iron phosphate, it can also be used to synthesize other olivine-type positive electrode materials, such as lithium manganese phosphate, lithium nickel phosphate, lithium cobalt phosphate, and cobalt silicate. Lithium, lithium iron silicate, lithium manganese silicate.
[0036] In the prepara...
Embodiment 1
[0042] 30mL of oleylamine was heated to 100°C under nitrogen protection and stirred. FeCl 2 , 1.014g dissolved in 15ml ethanol, LiAc·2H 2 After O, 0.816g was dissolved in 15ml of ethanol, they were added to the appeal of oleylamine. Add 1 mL of aniline and react at 100°C for 30 minutes. Add phosphoric acid mixture (0.55mL > 85% phosphoric acid + 5mL ethanol), react at 100°C for 2 hours, then raise the temperature from 100°C to 200°C. And maintained at 200 degrees for 4 hours. Cool to room temperature. Transfer out the reaction bottle, add ethanol to precipitate out. Then wash with a small amount of cyclohexane, then add ethanol to precipitate out. Wash twice. Then vacuum dry at 64°C overnight. Burn at 600°C for 4 hours under an argon atmosphere of 5% H2. to get the finished product. Such as figure 1 SEM characterization of the obtained product is shown. The charge-discharge curve at 0.5C is as follows figure 2 shown.
Embodiment 2
[0044] 60mL oleylamine was heated to 100°C under stirring, Mn(Ac) 2 4H 2 O, 3.92g dissolved in 25ml ethanol, LiAc·2H 2 After O, 1.632g was dissolved in 25ml of ethanol, they were added to the appeal of oleylamine. React at 100°C for 60 minutes. Add phosphoric acid mixture (1.1mL > 85% phosphoric acid + 8mL ethanol), react at 100°C for 2 hours, and then raise the temperature from 100°C to 200°C. And maintained at 200 degrees for 4 hours. Cool to room temperature. Transfer out the reaction bottle, add ethanol to precipitate out. Then wash with a small amount of cyclohexane, then add ethanol to precipitate out. Wash twice. Then vacuum dry at 64°C overnight. Under a nitrogen atmosphere, it was fired at 600° C. for 4 hours. to get the finished product. Such as image 3 Shown, its charge and discharge curve at 0.5C.
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