Method for preparing fused salt-oxalate co-precipitation of lithium-rich materials for lithium batteries

A lithium-rich material, molten salt technology, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of precipitation speed and particle size uniformity that are not easy to ensure, and achieve the stability of material structure, improve electrochemical performance, The effect of uniform particle size of the product

Inactive Publication Date: 2013-02-20
CHINA FIRST AUTOMOBILE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the basic salt co-precipitation method prepares the precursor, the uniformity of the precipitation speed and particle size is not easy to ensure

Method used

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  • Method for preparing fused salt-oxalate co-precipitation of lithium-rich materials for lithium batteries
  • Method for preparing fused salt-oxalate co-precipitation of lithium-rich materials for lithium batteries
  • Method for preparing fused salt-oxalate co-precipitation of lithium-rich materials for lithium batteries

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Preparation of Li[Li 0.33 Ni 0.33 mn 0.56 ]O 2 material, namely xLi 2 MnO 3 ( 1-x )LiMO 2 M=Ni in the material, x = 0.33. First, 9.693 g of Ni(NO 3 ) 2 and 9.941 g of Mn(NO 3 ) 2 Dissolve in 220 mL of deionized water to obtain solution A, and dissolve 6.75 g of oxalic acid in 150 mL of deionized water to obtain solution B. Take another beaker C, add 150 mL of deionized water, use ammonia water to control the pH at 8, and use a peristaltic pump to simultaneously drop liquids A and B into beaker C at a rate of 0.2 mL / min in a water bath at 40 °C. and stir vigorously. The obtained suspension was filtered, washed, and air-dried to obtain powder D. LiOH and LiNO with a molar mass ratio of 3.8:6.2 3 After grinding and mixing, heat it to 200°C to melt it, keep it warm for 1 hour, take out the crystal and grind it to get molten salt LiOH-LiNO 3 , coded as molten salt E. Mix 9.2921 g of molten salt E, 3.19 g of LiOH and D by ball milling to obtain mixture F. P...

Embodiment 2

[0028] Preparation of Li[Li 0.184 Ni 0.224 mn 0.725 ]O 2 material, namely x Li 2 MnO 3 ( 1-x )LiMO 2 M= Ni in the material 1 / 2 mn 1 / 2 , x = 0.45. First, 5.888 g of NiSO 4 and 12.253 g of MnSO 4 Dissolved in 120 mL deionized water to obtain solution A, 15g Na 2 C 2 o 4 Dissolve in 200 mL deionized water to obtain solution B. Use hydrochloric acid to control the pH value of solution B to be stable at 3, add solution A dropwise to solution B at a rate of 3 mL / min in a water bath at 80°C, and stir vigorously, filter the obtained suspension, wash and vacuum Powder C was obtained after drying. 34.79 g KCl, 8.152 g LiNO 3 Mix with ball mill C to get mixed powder D, put D into a resistance furnace, heat up to 600°C at a rate of 50°C per minute and keep it warm for 9 hours, then cool with the furnace, the resultant is washed repeatedly with deionized water and then baked at 60°C Dry to obtain the final product.

Embodiment 3

[0030] Preparation of Li[Li 0.167 Ni 0.166 co 0.166 mn 0.500 ]O 2 material, namely x Li 2 MnO 3 ( 1-x )LiMO 2 M= Ni in the material 1 / 3 co 1 / 3 mn 1 / 3 , x = 0.4. First, 4.13 g of Ni(CH 3 COO) 2 , 0.243 g of MnCl 2 and 4.135 g of Co(CH 3 COO) 2 Dissolved in 200 mL deionized water to obtain solution A, 26.8g K 2 C 2 o 4 Dissolve in 100 mL deionized water to obtain solution B. Under hydrothermal conditions at 65°C, use a peristaltic pump to drop B into solution A at a rate of 10 mL / min, while adjusting its pH to 6 with hydrochloric acid and stirring vigorously. The resulting suspension was filtered, washed and dried in vacuo to afford C. 44.06 g Li 2 CO 3 Mix and grind with powder C to obtain mixture D. Put D into a resistance furnace, raise the temperature to 900°C at a rate of 10°C per minute, keep it warm for 4 hours, and then cool it with liquid nitrogen. The resultant was washed several times with deionized water and then dried at 70°C to obtain t...

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Abstract

The invention discloses a method for preparing fused salt-oxalate co-precipitation of lithium-rich materials for lithium batteries. The method is characterized in that a Ni, Co and Mn metal salt solution and an oxalate root solution are prepared, and the two solutions are mixed together in different dropwise adding mode to form precipitation to serve as a precursor. The precursor, fused salt and lithium salt are mixed and sintered, resultants are cleaned and dried to obtain high-volume lithium-rich cathode materials x Li2MnO3*(1-x) LiMO2 (M=Co, Ni1 / 2 Mn1 / 2, Ni1 / 3Co1 / 3Mn1 / 3). When the lithium-rich materials are prepared, liquid environments of the fused salt are helpful for contact and reaction of the materials, and accordingly, reaction start time is reduced and reaction time is shortened. The oxalate is used as a precipitator, resultant particles are uniform, any impurity is not introduced, and the stability of material structures is facilitated and the electrochemical performance is improved.

Description

technical field [0001] The invention relates to a preparation method of molten salt-oxalate co-precipitation of lithium-rich materials for lithium batteries, in particular to a layered lithium-ion battery lithium-rich positive electrode material x Li 2 MnO 3 ( 1-x )LiMO 2 (M=Co, Ni, Ni 1 / 2 mn 1 / 2 、Ni 1 / 3 co 1 / 3 mn 1 / 3 ) The preparation method of combining molten salt and oxalate co-precipitation belongs to the technical field of lithium ion battery materials. Background technique [0002] Lithium-ion secondary batteries have been widely used in many fields such as portable electronic devices since their commercialization, and LiCoO 2 Due to the advantages of high voltage and stable electrochemical performance, it occupies an important position in the market. However, Co resources are relatively scarce and expensive, which limits its application; relatively cheap LiFePO 4 The ionic conductivity is poor, and the actual discharge specific capacity is only 160 mAhg ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/505H01M4/525
CPCY02E60/122Y02E60/10
Inventor 陈慧明姜涛张克金米新艳王丹魏哓川
Owner CHINA FIRST AUTOMOBILE
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