CN103050681A - Preparation method of high-compaction spherical ternary cathode material - Google Patents
Preparation method of high-compaction spherical ternary cathode material Download PDFInfo
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- CN103050681A CN103050681A CN2012105636546A CN201210563654A CN103050681A CN 103050681 A CN103050681 A CN 103050681A CN 2012105636546 A CN2012105636546 A CN 2012105636546A CN 201210563654 A CN201210563654 A CN 201210563654A CN 103050681 A CN103050681 A CN 103050681A
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Abstract
The invention relates to the preparation of a cathode active material of a lithium ion battery, in particular to a preparation method of a high-compaction spherical ternary cathode material. The preparation method is characterized by comprising the following steps: (1) firstly, synthesizing a precursor, wherein the specific step is that firstly deionized water, which is used as base solution, is added to a reaction kettle, and nickel salt, cobalt salt and manganese salt mixed solution, as well as an aqueous alkaline solution and a complexing agent is added into the reaction kettle at a volume ratio of (15-20):(15-20):1 at the same time; (2) stirring for performing surface treatment, and then performing filtrating to obtain a final precursor of the ternary cathode material after drying; and (3) uniformly mixing the obtained final precursor and lithium carbonate at a molar ratio of 1: (0.5-0.525) to be sintered and finally cooled. The method has the advantage that the preparation process can control the morphology and the particle size of the precursor, and is low in cost, non-pollution, and suitable for industrialized production.
Description
Technical field
The present invention relates to the preparation of anode active material of lithium ion battery, the preparation method of the spherical tertiary cathode material of especially high jolt ramming.
Background technology
Positive electrode is the important component part of lithium ion battery.At present the industrialization anode material for lithium-ion batteries be LiCoO
2, research and comparison is ripe, high comprehensive performance, but expensive, toxicity is larger, and there is defective in security performance, is especially overcharging under the condition, and material is unstable, and easy and electrolyte reacts, and application is a greater impact; In addition LiCoO
2Only have half lithium reversible embedding to take off, actual reversible capacity is about 145mAh/g, and the limiting lithium ion cell capacity improves, and can not satisfy the needs of the electrical source of power battery such as electric vehicle power sources, therefore needs to seek the new material of high-performance and low-cost.
In cobalt acid lithium substitution material, mainly contain LiFePO
4, LiMn
2O
4And LiNiO
2Deng, LiFePO wherein
4Have superior heat-stability and cyclicity, but actual capacitance low (＜140mAh/g), operating voltage low (3.4V), electron conduction be poor, high rate during charging-discharging is poor, restriction energy content of battery density; LiMn
2O
4Cost is low, and fail safe is good, but the especially high-risk poor performance of cycle performance, structural instability causes significant capacity attenuation; LiNiO
2Cost is low, and capacity is high, but the preparation difficulty, there are serious safety problem in the consistency of material property and poor reproducibility, all are difficult to satisfy the requirement that commercial lithium-ion batteries improves specific capacity and reduces cost.
At present, tertiary cathode material nickel, cobalt and manganese oxide system has the advantages such as cost is low, specific capacity is high, voltage platform is high, anti-excessively punching performance is good, good heat stability, and receives much concern.Studies show that this positive electrode concentrated LiCoO
2, LiMn
2O
4And LiNiO
2Separately advantage Deng material.
At present, synthesis of ternary positive electrode method is mainly high temperature solid-state method, exist three kinds of elements of nickel cobalt manganese to fail full and uniform mixing, fail to give full play to each self-applying, the synthetic material groups of grains becomes that bulk density is low, specific capacity is lower than the sour lithium of cobalt, therefore hinder the practical application of this material, improved practical significant to tertiary cathode material of the bulk density of tertiary cathode material and volume and capacity ratio.Lithium ion anode material bulk density, pattern, particle size and distribution, impurity content and tertiary cathode material precursor are closely related.Mostly the tertiary cathode material of present domestic report is to be formed by random sheet or granular solid matter, and bulk density is low, affected by the tertiary cathode material precursor, and the physical and chemical performance that improves precursor is particularly crucial to improving the tertiary cathode material performance.Main purpose of the present invention reaches the bulk density, processing characteristics, cycle performance and the thermal stability that improve tertiary cathode material by improving tertiary cathode material precursor physical and chemical performance, has more reduced the cost of ternary material.
Summary of the invention
The purpose of this invention is to provide the preparation method of the spherical tertiary cathode material of a kind of high jolt ramming, can reduce cost, reduce the pollution to environment, improve simultaneously the tertiary cathode material processing characteristics, overcome material capacity and Stable Defects.
The preparation method of the spherical tertiary cathode material of a kind of high jolt ramming, its special feature is, comprises the steps:
(1) at first synthesizes precursor, specifically first deionized water is added in the reactor as end liquid, then the mixing salt solution of nickel salt, cobalt salt, manganese salt and alkaline aqueous solution and complexing agent are 15-20: 15-20 by volume: 1 adds in the reactor simultaneously, wherein, the proportioning of nickel salt, cobalt salt, manganese salt and alkali is pressed chemical formula Ni
xCo
yMn
z(OH)
2Preparation, 0.3≤x in the formula≤1,0.1≤y≤0.5,0.1≤z≤0.5, and x+y+z=1; Then adopt the crystallization control method, the spherical tertiary cathode material precursor of synthesizing spherical or class, this precursor chemical formula is Ni
xCo
yMn
z(OH)
2, wherein 0.3≤x≤1,0.1≤y≤0.5,0.1≤z≤0.5, and x+y+z=1;
(2) add alkaline aqueous solution and transfer pH value 10～12, stir to carry out surface treatment, then filter, the raw material after filtering is carried out drying make the final precursor of tertiary cathode material;
The final precursor that (3) will obtain and lithium carbonate are 1 in molar ratio: (0.5～0.525) carries out even mixed sintering, sintering temperature is 550 ℃～680 ℃ and keeps 10h～16h, then be warming up to 800 ℃～900 ℃ and keep 5h～10h, cooling namely obtains tap density 〉=2.90g/cm at last
3Ternary material.
Nickel salt in the step (1), manganese salt, cobalt salt adopt sulfate, nitrate or the chlorate of nickel, manganese, cobalt, and the concentration of nickel salt, manganese salt, cobalt salt is controlled at 1.0～3.0mol/L in reaction solution.
Complexing agent adopts methyl-sulfoxide DMSO in the step (1).
Step (1) and (2) neutral and alkali aqueous solution are at least a among NaOH, KOH and the LiOH, and alkaline aqueous solution concentration is 2～6mol/L.
The crystallization control method specifically under argon gas, nitrogen or other inert gas shielding, is carried out the particle D50 to 5um after the continuous precipitation mode is controlled the sediment crystal growth in the step (1) in reactor.
After specifically being input to continuously in the eddy current type reactor with measuring pump nickel salt, cobalt salt, manganese salt solution, alkaline aqueous solution, methyl-sulfoxide in the step (1), solid content is 150～420mg/L in the control mother liquor, precipitation temperature is 50～80 ℃, the reactor mixing speed is 100～500rpm, the coprecipitation reaction time is 20～50 hours, pH value is controlled between 9.5～13.0, reactor feed liquid Natural excrement.
Solid content is controlled at 200～1300g/L in the course of reaction in the step (1).
After adding alkali in the step (2) and transferring PH to carry out surface treatment, carry out Separation of Solid and Liquid, again with deionized water washing Separation of Solid and Liquid gained solid product to the washings pH value less than till 9.
Drying in the step (2) refers to carry out drying 2～4 hours under 90 ℃～105 ℃.
Sulfur content is 800～1400ppm in the spherical tertiary cathode material precursor that obtains after the drying in the step (3).
The advantage of the inventive method is: in reactor, adopt the crystallization control technology, synthetic high densification, spherical tertiary cathode material precursor, this technique can be controlled pattern, the particle diameter of precursor, and it is simple, controlled that the method has, because complexing agent can be recycled by rectifying with methyl-sulfoxide (DMSO), so low, the pollution-free suitable suitability for industrialized production of cost.
Description of drawings
Fig. 1 is the Ni of the embodiment of the invention 1 preparation
1/3Co
1/3Mn
1/3(OH)
2The SEM distribution map of tertiary cathode material.
Embodiment
Embodiment 1:
With NiSO
4, MnSO
4, CoSO
4Ni:Mn:Co=1 in molar ratio: 1: 1 proportional arrangement nickel salt manganese salt cobalt salt mixed aqueous solution, total concentration is 3.0 mol/L, preparing in addition the sodium hydroxide solution of 6.0mol/L, 15: 15: 1 by volume was respectively that 97% DMSO solution is input to and fills with in advance 10cm with nickel, cobalt, manganese mixing salt solution, sodium hydroxide solution, purity with measuring pump again
3React in the reactor of deionized water.
Under the protective condition of argon gas, the control temperature of reaction kettle is 50 ℃, it is 11.0 that the flow of control alkali makes pH value, speed of agitator is 500r/min, solid content is 250mg/L in the control mother liquor, the feed liquid solid content is 450g/L in the control reactor, reactor feed liquid Natural excrement, continuous feed 30h stops charging, and material in the reactor is gone to ageing tank, the sodium hydroxide solution that adds again 3mol/L is transferred PH to 11.5, stir 2.0h and carry out surface treatment, then filter and carry out Separation of Solid and Liquid, with deionized water washing Separation of Solid and Liquid gained solid product to the washings pH value less than till 8; Then at 105 ℃ solid product is carried out dry 3h, dry spherical tertiary cathode material precursor as shown in Figure 1, product S content 1050ppm, pattern is spherical in shape.
(both are Powdered getting final product with prepared precursor and lithium carbonate, without the particle size range requirement, lower with) be in rotary furnace, to carry out sintering after mixing at 1: 0.5 in molar ratio, sintering temperature is 600 ℃ and keeps 12h, then is warming up to 850 ℃ and keeps 6h.The tap density that obtains ternary material behind the sintering is 2.95g/cm
3
Embodiment 2:
With Ni (NO
3)
2, Mn (NO
3)
2, Co (NO
3)
2Ni:Mn:Co=4 in molar ratio: 4: 2 ratio preparation nickel salt manganese salt cobalt salt mixed aqueous solutions, total concentration is 2.5mol/L, prepare again in addition the potassium hydroxide solution of 5mol/L, respectively with nickel, cobalt, manganese mixing salt solution, potassium hydroxide solution, purity were that 97% DMSO solution is input to and fills with in advance 10cm with measuring pump 15: 15: 1 by volume
3React in the reactor of deionized water.
Under the nitrogen protection condition, the control temperature of reaction kettle is 60 ℃, it is 10.5 that the flow of control alkali makes pH value, speed of agitator is 600r/min, solid content is 200mg/L in the control mother liquor, the feed liquid solid content is 400g/L in the control reactor, reactor feed liquid Natural excrement, continuous feed 25h stops charging, and material in the reactor is gone to ageing tank, the alkali that adds again 3mol/L is transferred pH value to 12.0, stir 2.0h and carry out surface treatment, filter and carry out Separation of Solid and Liquid, with deionized water washing Separation of Solid and Liquid gained solid product to the washings pH value less than till 8; Then at 105 ℃ solid product is carried out dry 2h and obtain spherical tertiary cathode material precursor, product S content 850ppm.
With prepared precursor and lithium carbonate be in molar ratio mix at 1: 0.525 after in rotary furnace sintering, sintering temperature is 650 ℃ and keeps 11h, 870 ℃ keep 6h.The tap density that obtains ternary material behind the sintering is 3.00g/cm
3
Embodiment 3:
With NiCl
2, MnCl
2, CoCl
2Ni:Mn:Co=5 in molar ratio: 3: 2 ratio preparation nickel salt manganese salt cobalt salt mixed aqueous solutions, total concentration is 2.5mol/L, preparing in addition the sodium hydroxide solution of 5mol/L, 15: 15: 1 by volume was respectively that 97% DMSO is input to and fills with in advance 10m with nickel, cobalt, manganese mixing salt solution, sodium hydroxide solution, purity with measuring pump again
3React in the reactor of deionized water.
Under the protective condition of helium; the control temperature of reaction kettle is 55 ℃; the flow of control alkali makes pH value 10.5; mixing speed is 550r/min; solid content is 260mg/L in the control mother liquor; the feed liquid solid content is 400g/L in the control reactor, reactor feed liquid Natural excrement, continuous feed 35h; stop charging; material in the reactor is gone to ageing tank, and the alkali that adds again 3mol/L is transferred PH to 12.0, stirs 2.0h and carries out surface treatment; then filter and carry out Separation of Solid and Liquid; with deionized water washing Separation of Solid and Liquid gained solid product to washings PH less than till 8.5, dry to spherical tertiary cathode material precursor, product S content 950ppm.
Be to carry out sintering after mixing at 1: 0.525 in rotary furnace in molar ratio with prepared precursor and lithium carbonate, sintering temperature is 650 ℃ and keeps 15h, and 870 ℃ keep 6h.The tap density that obtains ternary material behind the sintering is 2.93g/cm
3
Embodiment 4:
With NiSO
4, MnCl
2, CoSO
4In molar ratio Ni:Mn:Co=6:3:1 ratio preparation nickel salt manganese salt cobalt salt mixed aqueous solution, total concentration is 3.0mol/L, preparing in addition the sodium hydroxide solution of 6mol/L, is respectively that 97% DMSO is input to and fills with in advance 10m with nickel, cobalt, manganese mixing salt solution, sodium hydroxide solution, purity with measuring pump again
3React in the reactor of deionized water.
Under the protective condition of nitrogen; the control temperature of reaction kettle is 60 ℃; it is 11.0 that the flow of control alkali makes pH value; speed of agitator is 650r/min; solid content is 280mg/L in the control mother liquor; the feed liquid solid content is 420g/L in the control reactor, reactor feed liquid Natural excrement, continuous feed 32h; stop charging; material in the reactor is gone to ageing tank, and the alkali that adds again 3mol/L is transferred PH to 12.5 to stir 1.5h to carry out surface treatment, with deionized water washing Separation of Solid and Liquid gained solid product to the washings pH value less than till 8; then at 105 ℃ solid product is carried out dry 3h; drying obtains spherical tertiary cathode material precursor, product S content 1020ppm, and pattern is spherical in shape.
Be to carry out sintering after mixing at 1: 0.5 in rotary furnace in molar ratio with prepared precursor and lithium carbonate, sintering temperature is 650 ℃ and keeps 12h, and 870 ℃ keep 6h.The tap density that obtains ternary material behind the sintering is 2.92g/cm
3
Measure respectively tap density, the product S content of tertiary cathode material prepared in above-described embodiment 1～4, and list in the table 1 respectively.
| Embodiment | Chemical formula | Confirm density g/cm 3 | S(ppm) | Pattern |
| Embodiment 1 | LiNi 1/3Co 1/3Mn 1/3O 2 | 2.95 | 1050 | Spherical |
| Embodiment 2 | LiNi 0.4Co 0.4Mn 0.2O 2 | 3.00 | 850 | Spherical |
| Embodiment 3 | LiNi 0.5Co 0.3Mn 0.2O 2 | 2.93 | 950 | Spherical |
| Embodiment 4 | LiNi 0.6Co 0.3Mn 0.1O 2 | 2.92 | 1020 | Spherical |
Upper table 1 is example physical and chemical performance tables of data of the present invention.
Claims (10)
1. the preparation method of the one kind high spherical tertiary cathode material of jolt ramming is characterized in that, comprises the steps:
(1) at first synthesizes precursor, specifically first deionized water is added in the reactor as end liquid, then the mixing salt solution of nickel salt, cobalt salt, manganese salt and alkaline aqueous solution and complexing agent are 15-20: 15-20 by volume: 1 adds in the reactor simultaneously, wherein, the proportioning of nickel salt, cobalt salt, manganese salt and alkali is pressed chemical formula Ni
xCo
yMn
z(OH)
2Preparation, 0.3≤x in the formula≤1,0.1≤y≤0.5,0.1≤z≤0.5, and x+y+z=1; Then adopt the crystallization control method, the spherical tertiary cathode material precursor of synthesizing spherical or class, this precursor chemical formula is Ni
xCo
yMn
z(OH)
2, wherein 0.3≤x≤1,0.1≤y≤0.5,0.1≤z≤0.5, and x+y+z=1;
(2) add alkaline aqueous solution and transfer pH value 10～12, stir to carry out surface treatment, then filter, the raw material after filtering is carried out drying make the final precursor of tertiary cathode material;
The final precursor that (3) will obtain and lithium carbonate are 1 in molar ratio: (0.5～0.525) carries out even mixed sintering, sintering temperature is 550 ℃～680 ℃ and keeps 10h～16h, then be warming up to 800 ℃～900 ℃ and keep 5h～10h, cooling namely obtains tap density 〉=2.90g/cm at last
3Ternary material.
2. the preparation method of the spherical tertiary cathode material of high jolt ramming as claimed in claim 1, it is characterized in that: the nickel salt in the step (1), manganese salt, cobalt salt adopt sulfate, nitrate or the chlorate of nickel, manganese, cobalt, and the concentration of nickel salt, manganese salt, cobalt salt is controlled at 1.0～3.0mol/L in reaction solution.
3. the preparation method of the spherical tertiary cathode material of high jolt ramming as claimed in claim 1 is characterized in that: complexing agent employing methyl-sulfoxide DMSO in the step (1).
4. the preparation method of the spherical tertiary cathode material of high jolt ramming as claimed in claim 1 is characterized in that: step (1) and (2) neutral and alkali aqueous solution are at least a among NaOH, KOH and the LiOH, and alkaline aqueous solution concentration is 2～6mol/L.
5. the preparation method of the spherical tertiary cathode material of high jolt ramming as claimed in claim 1; it is characterized in that: the crystallization control method specifically under argon gas, nitrogen or other inert gas shielding, is carried out the particle D50 to 5um after the continuous precipitation mode is controlled the sediment crystal growth in the step (1) in reactor.
6. the preparation method of the spherical tertiary cathode material of high jolt ramming as claimed in claim 1, it is characterized in that: after specifically being input to continuously in the eddy current type reactor with measuring pump nickel salt, cobalt salt, manganese salt solution, alkaline aqueous solution, methyl-sulfoxide in the step (1), solid content is 150～420mg/L in the control mother liquor, precipitation temperature is 50～80 ℃, the reactor mixing speed is 100～500rpm, the coprecipitation reaction time is 20～50 hours, pH value is controlled between 9.5～13.0, reactor feed liquid Natural excrement.
7. the preparation method of the spherical tertiary cathode material of high jolt ramming as claimed in claim 6, it is characterized in that: solid content is controlled at 200～1300g/L in the course of reaction in the step (1).
8. the preparation method of the spherical tertiary cathode material of high jolt ramming as claimed in claim 1, it is characterized in that: after adding alkali in the step (2) and transferring PH to carry out surface treatment, carry out Separation of Solid and Liquid, again with deionized water washing Separation of Solid and Liquid gained solid product to the washings pH value less than till 9.
9. the preparation method of the spherical tertiary cathode material of high jolt ramming as claimed in claim 1, it is characterized in that: the drying in the step (2) refers to carry out drying 2～4 hours under 90 ℃～105 ℃.
10. the preparation method of the spherical tertiary cathode material of high jolt ramming as claimed in claim 1, it is characterized in that: sulfur content is 800～1400ppm in the spherical tertiary cathode material precursor that obtains after the drying in the step (3).
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106058244A (en) * | 2016-06-30 | 2016-10-26 | 广东省稀有金属研究所 | Preparation method and device of nickel-cobalt-aluminum anode material precursor |
| CN107623124A (en) * | 2017-09-30 | 2018-01-23 | 金驰能源材料有限公司 | A kind of preparation method of spherical nickel cobalt manganese persursor material |
| CN109346726A (en) * | 2018-11-12 | 2019-02-15 | 合肥斯姆雷品牌管理有限公司 | A kind of high temperature modification manganese systems lithium battery anode |
| CN109360983A (en) * | 2018-10-29 | 2019-02-19 | 合肥国轩高科动力能源有限公司 | Modified high-nickel ternary cathode material and preparation method and application thereof |
| CN110817976A (en) * | 2019-10-25 | 2020-02-21 | 合肥国轩高科动力能源有限公司 | Positive electrode material precursor and preparation method and application thereof |
| CN112687868A (en) * | 2020-12-28 | 2021-04-20 | 大连博融新材料有限公司 | High-nickel ternary cathode material and preparation method thereof |
| CN113451565A (en) * | 2021-05-06 | 2021-09-28 | 福建常青新能源科技有限公司 | Production process of high-tap-density high-sphericity internal radial ternary precursor |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106058244A (en) * | 2016-06-30 | 2016-10-26 | 广东省稀有金属研究所 | Preparation method and device of nickel-cobalt-aluminum anode material precursor |
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| CN109360983B (en) * | 2018-10-29 | 2021-08-06 | 合肥国轩高科动力能源有限公司 | Modified high-nickel ternary cathode material and preparation method and application thereof |
| CN109346726A (en) * | 2018-11-12 | 2019-02-15 | 合肥斯姆雷品牌管理有限公司 | A kind of high temperature modification manganese systems lithium battery anode |
| CN109346726B (en) * | 2018-11-12 | 2020-10-30 | 合肥斯姆雷品牌管理有限公司 | High-temperature manganese lithium battery anode |
| CN110817976A (en) * | 2019-10-25 | 2020-02-21 | 合肥国轩高科动力能源有限公司 | Positive electrode material precursor and preparation method and application thereof |
| CN110817976B (en) * | 2019-10-25 | 2022-05-17 | 合肥国轩高科动力能源有限公司 | Positive electrode material precursor and preparation method and application thereof |
| CN112687868A (en) * | 2020-12-28 | 2021-04-20 | 大连博融新材料有限公司 | High-nickel ternary cathode material and preparation method thereof |
| CN113451565A (en) * | 2021-05-06 | 2021-09-28 | 福建常青新能源科技有限公司 | Production process of high-tap-density high-sphericity internal radial ternary precursor |
| CN113451565B (en) * | 2021-05-06 | 2024-02-13 | 福建常青新能源科技有限公司 | Production process of high-tap high-sphericity internal radial ternary precursor |
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