Method used for preparing nickel-based layer structural ternary cathode material using microwave

A technology of ternary materials and positive electrode materials, which is applied in the direction of structural parts, electrical components, battery electrodes, etc., to achieve the effects of low energy consumption, shortened process flow, and reduced energy consumption

Inactive Publication Date: 2014-03-26
江西省钨与稀土产品质量监督检验中心(江西省钨与稀土研究院)
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  • Abstract
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Problems solved by technology

[0007] In order to overcome the deficiencies of the existing lithium-ion batteries, the present invention provides a nickel-based layered structure LiNi battery prepared by microwave synthesis, drying and sintering. x co y mn 1-x-y o 2 The method of ternary positive electrode materials, using the complexati

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation of step 1 feed liquid:

[0027] (1) Add 0.02molNiSO 4 ·6H 2 O, 0.012molCoSO 4 ·7H 2 O, 0.008molMnSO 4 ·H 2 O was dissolved in 140ml of a mixture of deionized water and isopropanol, wherein isopropanol accounted for 10% of the volume of the mixture. Stir at room temperature and normal pressure until completely dissolved, and the molar ratio of Ni:Co:Mn after dissolution is 5:3:2.

[0028] (2) Add 0.044mol of (NH 4 ) 2 C 2 o 4 ·H 2 Dissolve O in 60 ml of a mixture of deionized water and isopropanol, in which isopropanol accounts for 10% of the volume of the mixture, stir at 60°C under normal pressure until it is completely dissolved, and hold the ammonium oxalate solution Keep the container tightly closed to reduce the evaporation of water.

[0029] Step 2 Co-precipitation reaction: After the above-mentioned heated ammonium oxalate solution is completely dissolved, it is quickly poured into the ternary mixture solution, heated by microwave at 6...

Embodiment 2

[0033] (1) Add 0.03molNi(NO 3 ) 2 ·6H 2 O, 0.018molCo(NO 3 ) 2 ·6H 2 O, 0.024molMn(NO 3 ) 2 (50% solution) was dissolved in a mixture of 120ml of deionized water and absolute ethanol, wherein absolute ethanol accounted for 20% of the volume of the mixture. Stir at room temperature until completely dissolved, and the molar ratio of Ni:Co:Mn after dissolution is 5:3:2.

[0034] (2) Add 0.066mol of Na 2 C 2 o 4 Dissolve in a mixture of 180 ml of deionized water and absolute ethanol, of which absolute ethanol accounts for 20% of the volume of the mixture, heat and stir at 70°C until completely dissolved, and seal the container holding the sodium oxalate solution to reduce water evaporation quantity.

[0035] (3) After the above-mentioned heated sodium oxalate solution is completely dissolved, quickly pour the ternary mixture into the sodium oxalate solution, heat with microwave at 75°C and stir for 20 minutes.

[0036] (4) After aging the above-mentioned co-precipitat...

Embodiment 3

[0039] (1) Add 0.05molNiCl 2 ·6H 2 O, 0.03mol CoCl 2 ·6H 2 O, 0.02molMnCl 2 4H 2 O was dissolved in a mixture of 250ml of deionized water and ethylene glycol, wherein ethylene glycol accounted for 15% of the volume of the mixture. Stir at room temperature until completely dissolved, and the molar ratio of Ni:Co:Mn after dissolution is 5:3:2.

[0040] (2) Add 0.11mol of K 2 C 2 o 4 ·H 2 Dissolve O in a mixture of 250 ml deionized water and ethylene glycol, where ethylene glycol accounts for 15% of the volume of the mixture, stir at 60°C until completely dissolved, and seal the container holding the potassium oxalate solution to reduce water evaporation quantity.

[0041] (3) After the above-mentioned heated potassium oxalate solution is completely dissolved, quickly pour it into the ternary mixture, heat to 90°C with microwave and stir for 10 minutes.

[0042] (4) After aging the above-mentioned co-precipitation reaction mixture for 10 minutes, separate the solid and...

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Abstract

The invention discloses a method used for preparing a nickel-based layer structural ternary cathode material via microwave synthesis, drying and sintering. The method is characterized in comprising following steps: (1) a ternary nickel, cobalt, manganese salt and oxalate water-alcohol mixed solution is prepared according to a ratio; (2) an oxalate solution and the ternary mixed solution are mixed rapidly, and are subjected to microwave heating and stirring; (3) a coprecipitate is filtered, washed and subjected to vacuum drying; (4) the dried coprecipitate is mixed with a lithium salt, and a mixed material is grinded, and is subjected to high-temperature solid phase reaction in a microwave sintering furnace so as to obtain the layer structural LiNixCoyMn1-x-yO2 (x=0.5, y=0.2 or 0.3) cathode material. According to the method, oxalate in ammonium oxalate possesses complexing performance, and is capable of realizing coprecipitation with nickel, cobalt and manganese via ternary complexing; the ternary cathode material is obtained via microwave synthesis and sintering; first charge discharge efficiency is more than 90%; 0.2C discharge capacity is more than 155mAh/g; and cycling performance is excellent.

Description

technical field [0001] The invention belongs to the technical field of new energy materials, and relates to a method of microwave synthesis, drying and sintering to prepare nickel-based layered structure LiNi x co y mn 1-x-y o 2 (X=0.5, Y=0.2 or 0.3) The method of ternary cathode material. Background technique [0002] Lithium-ion batteries have the advantages of small size, light weight, high voltage, high specific capacity, long cycle life, no memory effect, small self-discharge and low pollution. Since the 1990s, commercial lithium-ion batteries have been widely used in Portable products such as mobile phones, digital cameras, and notebook computers, as well as medical equipment, automobiles, and aerospace fields. In recent years, with the general reduction in the price of electronic products, the consumption of lithium-ion batteries has increased sharply. At present, my country is the world's largest producer, consumer and exporter of lithium batteries. [0003] As ...

Claims

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Application Information

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IPC IPC(8): H01M4/505H01M4/525
CPCY02E60/122H01M4/505H01M4/525H01M10/0525Y02E60/10
Inventor 姚文俐卢博
Owner 江西省钨与稀土产品质量监督检验中心(江西省钨与稀土研究院)
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