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Method for preparing lithium-enriched lithium manganese oxide solid solution cathode material

A lithium-rich lithium manganese oxide and positive electrode material technology, which is applied in battery electrodes, electrical components, circuits, etc., can solve the limitations of lithium-rich lithium manganate solid solution positive electrode material composition, affect product performance and consistency, and raw material ratio deviation, etc. problems, to achieve the effects of not being easily oxidized and deteriorated, reducing the cost of preparation, and determining and reliable composition

Active Publication Date: 2012-07-04
HUBEI WANRUN NEW ENERGY TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] 1. In order to ensure the uniform co-precipitation of the three ions of nickel, cobalt and manganese, a certain complexing agent must be used, and even multiple complexing agents must be used at the same time, which significantly increases the cost;
[0013] 2. Divalent manganese ions are easily oxidized when forming hydroxide precipitates. Inert gas protection is required during preparation, and oxidation should also be prevented during drying. Otherwise, the ratio of raw materials will be deviated during subsequent batching, which will affect product performance and consistency. ;
[0014] 3. Due to the different complexing abilities of complexing agents to nickel, cobalt, and manganese, and the different solubility products of hydroxides, it is difficult to flexibly adjust the composition of products in a wide range by the hydroxide co-precipitation method, resulting in the preparation of The composition of lithium-rich lithium manganese oxide solid solution cathode material is greatly restricted;
[0016] At present, there is no report on the preparation of lithium-rich lithium manganese oxide solid solution positive electrode materials by oxalate co-precipitation-high temperature solid phase method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Ammonium oxalate (NH 4 ) 2 C 2 o 4 3 liters of aqueous solution, that is, dissolve 380.11 grams of oxalic acid H in hot deionized water at about 60 ° C 2 C 2 o 4 .2H 2 0, add 500 milliliters of strong ammonia water of 12M again, be settled to 3 liters.

[0049] Prepare 1 / 6M nickel sulfate NiSO 4 , 1 / 6M cobalt sulfate CoSO 4 , 4 / 6M manganese sulfate MnSO 4 Mix 3 liters of aqueous solution.

[0050] Add 3 liters of ammonium oxalate solution into a glass reactor with a volume of 7 liters, stir vigorously, and pour constant temperature water into the jacket of the reactor to control the temperature of the materials in the reactor to 59-61°C.

[0051] Continuously input the mixed aqueous solution of nickel sulfate, cobalt sulfate and manganese sulfate into the reaction kettle with a peristaltic pump, control the flow rate to 50 ml / min, complete the feeding in about 1 hour, and continue to stir and age for 2 hours. During this process, the temperature of the react...

Embodiment 2

[0059] Prepare sodium oxalate Na at a concentration of 0.1M 2 C 2 o 4 3 liters of aqueous solution, that is, dissolve 38.01 grams of oxalic acid H in hot deionized water at about 60 ° C 2 C 2 o 4 .2H 2 O and 24 grams of sodium hydroxide NaOH, make up to 3 liters.

[0060] Prepare 0.02M nickel chloride NiCl 2 , 0.01M Cobalt Chloride CoCl 2 , 0.07M manganese chloride Mn Cl 2 Mix 3 liters of aqueous solution.

[0061] Add 3 liters of sodium oxalate solution into a glass reaction kettle with a volume of 7 liters, stir vigorously, and pour constant temperature water into the jacket of the reaction kettle to control the temperature of the materials in the reaction kettle to 96-98°C.

[0062] Continuously input the mixed aqueous solution of nickel chloride, cobalt chloride and manganese chloride into the reaction kettle with a peristaltic pump, control the flow rate to 50 ml / min, complete the feeding in about 1 hour, and continue to stir and age for 2 hours. During this pr...

Embodiment 3

[0070] Ammonium oxalate (NH 4 ) 2 C 2 o 4 3 liters of aqueous solution, that is, dissolve 570.17 grams of oxalic acid H in hot deionized water at about 80 ° C 2 C 2 o 4 .2H 2 0, add 750 milliliters of strong ammonia water of 12M again, be settled to 3 liters.

[0071] Prepare 0.375M nickel nitrate Ni(NO 3 ) 2 , 0.150M cobalt nitrate Co(NO 3 ) 2 , 0.975M manganese nitrate Mn(NO 3 ) 2 Mix 3 liters of aqueous solution.

[0072] Add 3 liters of ammonium oxalate solution into a glass reaction kettle with a volume of 7 liters, stir vigorously, and pour constant temperature water into the jacket of the reaction kettle to control the temperature of the materials in the reaction kettle to 79-81°C.

[0073] Continuously input the mixed aqueous solution of nickel nitrate, cobalt nitrate and manganese nitrate into the reaction kettle with a peristaltic pump, control the flow rate to 50 ml / min, complete the feeding in about 1 hour, and continue to stir and age for 2 hours. D...

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Abstract

The invention relates to a method for preparing a lithium-enriched lithium manganese oxide solid solution cathode material. The method comprises the following steps of: adding a mixed aqueous solution of nickel salt, cobalt salt and manganese salt into an oxalic acid or oxalate aqueous solution by an oxalate coprecipitation high-temperature solid state method, and stirring and reacting to generate nickel, cobalt and manganese oxalate coprecipitation; performing solid and liquid separation, washing and drying to obtain a nickel, cobalt and manganese oxalate precursor; and mixing and grinding the precursor and lithium salt, drying, baking at high temperature in an air atmosphere, and thus obtaining the lithium-enriched lithium manganese oxide solid solution cathode material. During preparation of the precursor, the proportion of the nickel salt, the cobalt salt and the manganese salt is adjusted, so that the constituents of the lithium-enriched lithium manganese oxide solid solution cathode material can be adjusted flexibly. The preparation method is suitable for large-scale, economic, stable and reliable production of the lithium-enriched lithium manganese oxide solid solution cathode material, has obvious advantages, and is high in practical value.

Description

technical field [0001] The invention belongs to the technical field of energy material preparation, and relates to a lithium-rich lithium manganate solid solution positive electrode material (Li 2 MnO 3 -LiMO 2 , M is at least one of Ni, Co, and Mn), the material is a new type of high-voltage, high-capacity lithium-ion battery positive electrode material. Background technique [0002] Lithium-ion batteries have been widely used in electronic products such as mobile phones, notebook computers, and digital cameras, and are developing into large-scale power batteries (such as for electric vehicles) and energy storage batteries (such as for solar and wind power generation systems). The pursuit of high energy density is an important goal in the development of lithium-ion batteries. [0003] The core of lithium-ion batteries is materials, including positive electrode materials, negative electrode materials, separators, electrolytes, etc. At present, the practical cathode mate...

Claims

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Application Information

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IPC IPC(8): H01M4/505H01M4/525
CPCY02E60/122Y02E60/10
Inventor 应皆荣刘世琦
Owner HUBEI WANRUN NEW ENERGY TECH DEV
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