CN107500366A - The preparation method of high performance spherical nickel cobalt lithium aluminate cathode material - Google Patents
The preparation method of high performance spherical nickel cobalt lithium aluminate cathode material Download PDFInfo
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- CN107500366A CN107500366A CN201710767839.1A CN201710767839A CN107500366A CN 107500366 A CN107500366 A CN 107500366A CN 201710767839 A CN201710767839 A CN 201710767839A CN 107500366 A CN107500366 A CN 107500366A
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- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- H—ELECTRICITY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The present invention relates to the preparation method of high performance spherical nickel cobalt lithium aluminate cathode material.Comprise the following steps：Aluminium salt is dissolved in sodium hydroxide solution；Prepare nickel salt aqueous solution, cobalt salt solution；Acetylacetone,2,4-pentanedione, nickel cobalt salt complexing agent ammonia spirit, precipitant solution are standby.Above-mentioned solution is added in reactor simultaneously, control aluminium, nickel, cobalt mole add, and control aluminium salt and the mol ratio of acetylacetone,2,4-pentanedione, the mol ratio of nickel cobalt salt and nickel cobalt complexing agent.At 30 80 DEG C, continue 20 80h, 10 20h of ageing reaction.Reaction solution centrifugal filtration is obtained into a filter cake, filter cake is added into sodium carbonate liquor to be followed by stirring and washing, then carry out centrifugal filtration and obtain secondary filter cake, secondary filter cake is then carried out repeatedly into washing and filtering using distilled water, to filtrate pH ＜ 9, obtains final filter cake.Final filtration cakes torrefaction obtains presoma.Presoma is mixed into lithium and sinters to obtain nickel cobalt lithium aluminate cathode material after oxygen in revolution sintering furnace.
Description
Technical field
The present invention relates to the preparation method of high performance spherical nickel cobalt lithium aluminate cathode material, belongs to lithium battery manufacturing field.
Background technology
Lithium ion battery as a kind of new battery, have voltage it is high, it is bigger than energy, have extended cycle life, discharge performance
Stably, the advantages that security is good, pollution-free and operating temperature range is wide, lithium ion battery is because of its excellent characteristic and by very big
Pay attention to.But the positive electrode of lithium ion battery is much lower compared to the specific capacity of negative material, this is answered now to improve lithium-ion electric
The approach of the specific capacity in pond is exactly positive electrode.
The positive electrode having been commercialized at present mainly has cobalt acid lithium, LiFePO4, LiMn2O4 and ternary material etc..Cobalt acid lithium
Positive electrode is earliest commercialized lithium ion battery, although its energy density is high, its cost is high, and environmental pollution also compares
Greatly；Manganate cathode material for lithium cost is low, safe, but its specific capacity is low and high-temperature behavior is poor；Ferrous lithium phosphate cathode
Material price is moderate, and cycle performance is very good, but cryogenic property is bad, and energy density per unit volume is relatively low.Make a general survey of main at present several
Positive electrode, the unique advantage of nickel cobalt lithium aluminate cathode material display, has assembled three kinds of cobalt acid lithium, LiMn2O4 and lithium nickelate positive poles
The advantages of material, i.e. high-energy, high power capacity, high security etc., charge and discharge platform is close with cobalt acid lithium, it is considered to be most possible
Cobalt acid lithium and one of commercialized positive electrode are substituted, and the success of tesla's electric car also demonstrate that its practicality.
The traditional preparation method of nickel cobalt aluminic acid lithium material is：Nickel cobalt aluminum complex hydroxide is first prepared using coprecipitation
Or carbonate deposition, then after this presoma is mixed by a certain percentage with lithium source, formed in oxygen atmosphere high temperature sintering.This method exists
When nickel cobalt aluminium is co-precipitated, due to the introducing of aluminium, it is precipitated, and solubility product is larger in nickel cobalt difference and aluminium has both sexes, is easily caused particle
Spherical morphology is deteriorated, and Elemental redistribution is uneven etc..Use saggar solid state sintering more during sintering, easily cause the poor quality opposite sex.
It is therefore desirable to improve the preparation method of nickel cobalt lithium aluminate to improve the performance of nickel cobalt lithium aluminate cathode material.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies in the prior art, there is provided a kind of high performance spherical nickel cobalt aluminium
The preparation method of sour lithium anode material, using the special process being complexed again to the aluminium element alkali soluble in material, preferably realize
Each element co-precipitation.The nickel cobalt lithium aluminate Elemental redistribution prepared using this method is uniform, and impurity content is low, and product is consistent
Property good, excellent performance and technological process is simple, suitable for large-scale production.
The purpose of the present invention is achieved through the following technical solutions：
The method for preparing anode material of high performance spherical nickel cobalt lithium aluminate, its described molecular formula are LiNixCoyAl1-x-yO2, it is special
Sign is, specifically includes following steps：
（1）A certain amount of aluminium salt is weighed, stirring and dissolving is standby as solution A after a certain amount of sodium hydroxide solution；Prepare nickel
Saline solution is standby as solution C as solution B, cobalt salt solution；Another configuration aluminium salt complexing agent acetylacetone,2,4-pentanedione solution D, nickel cobalt salt
Complexing agent ammonia spirit E, precipitant solution F are standby.
（2）Solution A, B, C, D, E, F are added in CSTR reactors simultaneously, control A, B, C solution is according to stoichiometry
The nickel cobalt aluminium mole of ratio adds, while controls aluminium salt and the mol ratio of acetylacetone,2,4-pentanedione, mole of nickel cobalt salt and nickel cobalt complexing agent
Than.Under conditions of 30-80 DEG C, persistently feed 20-80h, and charging carries out ageing reaction 10-20h after terminating.
（3）After reaction solution is carried out into centrifugal filtration, a filter cake is obtained, a filter cake is added into certain density sodium carbonate
Solution is followed by stirring and washing, and then carries out centrifugal filtration and obtains secondary filter cake, then carries out secondary filter cake repeatedly using distilled water
Washing and filtering obtains final filter cake to filtrate pH ＜ 9.
（4）Final filter cake is dried under vacuum state and both obtains spherical nickel-cobalt aluminium hydroxide presoma.
（5）Will nickel cobalt aluminium presoma mix lithium after be placed in revolution sintering furnace in, be passed through oxygen atmosphere be sintered both nickel cobalt
Lithium aluminate cathode material.
Further, step（1）Described in aluminium salt be aluminum nitrate, aluminium hydroxide or aluminum oxide in one or more.Nickel
Salt, cobalt salt are the one or more in its nitrate, sulfate, acetate.Precipitating reagent F is sodium hydroxide, sodium carbonate, hydroxide
One or more in potassium, lithium hydroxide.
Further, step（1）Described in the aluminium element in material use the special process that is complexed again of first alkali soluble,
First aluminium salt is dissolved in a certain amount of sodium hydroxide solution, then is complexed with aluminium salt complexing agent special acetylacetone,2,4-pentanedione solution
Reaction.
Further, step（1）Described in acetylacetone,2,4-pentanedione solution D concentration be mass fraction 1-3%.
Further, step（2）Described in aluminium salt and the mol ratio of acetylacetone,2,4-pentanedione be 1:0.5-1:2, nickel cobalt salt and ammoniacal liquor
Mol ratio be 1:0.5-1:2.
Further, step（3）Described in concentration of sodium carbonate be mass fraction 1-5%.
Further, step（4）Described in drying condition be to be carried out under vacuum state, and vacuum level requirements are 0.08-
0.1Mpa。
Further, step（5）Described in turn round sintering furnace burner hearth material be titanium alloy.
The present invention is had the following advantages relative to prior art and effect：First alkali soluble is used again to the aluminium element in material
The special process of complexing, preferably realize each element co-precipitation.The nickel cobalt lithium aluminate Elemental redistribution of preparation is uniform, impurity member
Cellulose content is low, good product consistency, excellent performance and technological process is simple, suitable for large-scale production.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of nickel cobalt lithium aluminate prepared by the embodiment of the present invention 1.
Fig. 2 is the first charge-discharge curve map of nickel cobalt lithium aluminate prepared by the embodiment of the present invention 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of nickel cobalt lithium aluminate prepared by the embodiment of the present invention 2.
Fig. 4 is the first charge-discharge curve map of nickel cobalt lithium aluminate prepared by the embodiment of the present invention 2.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Embodiment 1:
The water aluminum nitrates of 500g nine are weighed, stirring and dissolving is in 13kg sodium hydroxide solutions；Weigh 5.6kg nickel sulfates and be dissolved in 10kg distillations
Water；Weigh 1.15kg cobaltous sulfates and be dissolved in 5kg distilled water；Configure 0.2mol/L acetylacetone,2,4-pentanedione solution；5mol/L ammonia spirits；
4mol/L sodium hydroxide solutions are standby.
By above-mentioned each solution, cocurrent is added in CSTR reactors simultaneously, and it is 0.8 to control nickel cobalt al mole ratio:0.15:
0.05, while it is 1 to control the mol ratio of aluminum salt solution and acetylacetone,2,4-pentanedione:0.3, the mol ratio of nickel cobalt salt and ammoniacal liquor is 1:1.40
Under conditions of DEG C, persistently feed 40h, and charging carries out ageing reaction 10h after terminating.After reaction solution is carried out into centrifugal filtration, obtain
Filter cake, the sodium carbonate liquor that a filter cake adds mass fraction 2% is followed by stirring and washing, and is then carried out centrifugal filtration and is obtained
Secondary filter cake, secondary filter cake is then subjected to repeatedly washing and filtering using distilled water and, to filtrate pH ＜ 9, obtains final filter cake.Yu Zhen
The lower 120 DEG C of dryings of dummy status both obtain spherical nickel-cobalt aluminium hydroxide presoma.Revolution burning is placed in after nickel cobalt aluminium presoma is mixed into lithium
In freezing of a furnace, be passed through 800 DEG C of oxygen be sintered 15h both nickel cobalt lithium aluminate cathode material.
Embodiment 2:
110g aluminum hydroxide solids are weighed, stirring and dissolving is in 12kg sodium hydroxide solutions；Weigh 5.35kg nickel sulfates and be dissolved in 9.8kg
Distilled water；Weigh 1.26kg cobaltous sulfates and be dissolved in 5.3kg distilled water；Configure 0.2mol/L acetylacetone,2,4-pentanedione solution；5mol/L ammoniacal liquor is molten
Liquid；4mol/L sodium hydroxide solutions are standby.
By above-mentioned each solution, cocurrent is added in CSTR reactors simultaneously, and it is 0.75 to control nickel cobalt al mole ratio:0.15:
0.1 adds, while it is 1 to control the mol ratio of aluminum salt solution and acetylacetone,2,4-pentanedione:0.4, the mol ratio of nickel cobalt salt and ammoniacal liquor is 1:1.
Under conditions of 50 DEG C, persistently feed 30h, and charging carries out ageing reaction 10h after terminating.After reaction solution is carried out into centrifugal filtration,
A filter cake is obtained, the sodium carbonate liquor that a filter cake adds mass fraction 3% is followed by stirring and washing, then carries out centrifuging
Secondary filter cake is filtered to obtain, secondary filter cake is then carried out repeatedly into washing and filtering using distilled water, to filtrate pH ＜ 9, obtains final filter cake.
Spherical nickel-cobalt aluminium hydroxide presoma is both obtained in the lower 120 DEG C of dryings of vacuum state.It is placed in back after nickel cobalt aluminium presoma is mixed into lithium
Turn in sintering furnace, be passed through 780 DEG C of oxygen be sintered 20h both nickel cobalt lithium aluminate cathode material.
Embodiment 3:
The water aluminum nitrate aluminium of 1.0kg nine is weighed, stirring and dissolving is in 18kg sodium hydroxide solutions；Weigh 12.3kg nickel sulfates and be dissolved in 21kg
Distilled water；Weigh 2.4kg cobaltous sulfates and be dissolved in 10kg distilled water；Configure 0.3mol/L acetylacetone,2,4-pentanedione solution；10mol/L ammoniacal liquor is molten
Liquid；4mol/L sodium hydroxide solutions are standby.
By above-mentioned each solution, cocurrent is added in CSTR reactors simultaneously, and it is 0.8 to control nickel cobalt al mole ratio:0.15:
0.05, while it is 1 to control the mol ratio of aluminum salt solution and acetylacetone,2,4-pentanedione:0.4, the mol ratio of nickel cobalt salt and ammoniacal liquor is 1:0.5.
Under conditions of 40 DEG C, persistently feed 80h, and charging carries out ageing reaction 12h after terminating.After reaction solution is carried out into centrifugal filtration, take
A filter cake is obtained, the sodium carbonate liquor that a filter cake adds mass fraction 5% is followed by stirring and washing, then carries out centrifugal filtration
Secondary filter cake is obtained, secondary filter cake is then carried out repeatedly into washing and filtering using distilled water, to filtrate pH ＜ 9, obtains final filter cake.In
The lower 120 DEG C of dryings of vacuum state both obtain spherical nickel-cobalt aluminium hydroxide presoma.Revolution is placed in after nickel cobalt aluminium presoma is mixed into lithium
In sintering furnace, be passed through 760 DEG C of oxygen be sintered 20h both nickel cobalt lithium aluminate cathode material.
Claims (8)
1. a kind of preparation method of high performance spherical nickel cobalt lithium aluminate cathode material, the molecular formula of the nickel cobalt lithium aluminate are
LiNixCoyAl1-x-yO2, it is characterised in that specifically include following steps：
Weigh aluminium salt stirring and dissolving and solution A is used as after sodium hydroxide solution；Nickel salt solution is prepared as solution B, cobalt salt solution
As solution C；It is standby to configure acetylacetone,2,4-pentanedione solution D, ammonia spirit E, precipitant solution F；
By solution A, B, C, D, E and F simultaneously be added in CSTR reactors, A, B, C solution according to stoichiometric proportion nickel cobalt aluminium
Mole adds, while controls the mol ratio of aluminium salt and acetylacetone,2,4-pentanedione solution D, the mol ratio of nickel cobalt salt and ammonia spirit E,
Under conditions of 30-80 DEG C, persistently feed 20-80h, and charging carries out ageing reaction 10-20h after terminating；
After reaction solution is carried out into centrifugal filtration, a filter cake is obtained, a filter cake is added into sodium carbonate liquor is followed by stirring and washing,
Then carry out centrifugal filtration and obtain secondary filter cake, secondary filter cake is then subjected to repeatedly washing and filtering to filtrate pH ＜ using distilled water
9, obtain final filter cake；
Final filter cake is dried under vacuum state and both obtains spherical nickel-cobalt aluminium hydroxide presoma,
Will nickel cobalt aluminium presoma mix lithium after be placed in revolution sintering furnace in, be passed through oxygen atmosphere be sintered both nickel cobalt lithium aluminate just
Pole material.
2. the preparation method of the high performance spherical nickel cobalt lithium aluminate cathode material according to claim 1, it is characterised in that：
The aluminium salt is the one or more in aluminum nitrate, aluminium hydroxide or aluminum oxide, and nickel salt, cobalt salt are its nitrate, sulfate, vinegar
One or more in hydrochlorate, precipitant solution F are sodium hydroxide, sodium carbonate, potassium hydroxide, one kind in lithium hydroxide or several
Kind.
3. the preparation method of the high performance spherical nickel cobalt lithium aluminate cathode material according to claim 1, it is characterised in that：
Aluminium salt is first dissolved in alkaline solution sodium hydroxide solution, then by acetylacetone,2,4-pentanedione complex reaction, i.e., aluminium salt first is dissolved in into hydroxide
In sodium solution, then with aluminium salt complexing agent special acetylacetone,2,4-pentanedione solution carry out complex reaction.
4. the preparation method of the high performance spherical nickel cobalt lithium aluminate cathode material according to claim 1, it is characterised in that：
The acetylacetone,2,4-pentanedione solution D concentration is mass fraction 1-3%.
5. the preparation method of the high performance spherical nickel cobalt lithium aluminate cathode material according to claim 1, it is characterised in that：
The aluminium salt and the mol ratio of acetylacetone,2,4-pentanedione are 1:0.5-1:2, the mol ratio of nickel cobalt salt and ammoniacal liquor is 1:0.5-1:2.
6. the preparation method of the high performance spherical nickel cobalt lithium aluminate cathode material according to claim 1, it is characterised in that：
The concentration of sodium carbonate is mass fraction 1-5%.
7. the preparation method of the high performance spherical nickel cobalt lithium aluminate cathode material according to claim 1, it is characterised in that
（The drying condition is to be carried out under vacuum state, and vacuum level requirements are 0.08-0.1Mpa.
8. the preparation method of the high performance spherical nickel cobalt lithium aluminate cathode material according to claim 1, it is characterised in that
Described in turn round sintering furnace burner hearth material be titanium alloy.
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Cited By (1)
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| CN111430706A (en) * | 2019-11-29 | 2020-07-17 | 蜂巢能源科技有限公司 | Method for washing high-nickel carbonate precursor material and high-nickel carbonate precursor material |
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Application publication date: 20171222 |