CN102938459A - Method for preparing positive material of high-power lithium ion battery - Google Patents

Method for preparing positive material of high-power lithium ion battery Download PDF

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CN102938459A
CN102938459A CN2012104584949A CN201210458494A CN102938459A CN 102938459 A CN102938459 A CN 102938459A CN 2012104584949 A CN2012104584949 A CN 2012104584949A CN 201210458494 A CN201210458494 A CN 201210458494A CN 102938459 A CN102938459 A CN 102938459A
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template
preparation process
lithium ion
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CN102938459B (en
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王盈来
姜应律
张欣瑞
杨国凯
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Zhejiang Nandu Hongxin Power Technology Co.,Ltd.
Zhejiang Narada Power Source Co Ltd
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HANGZHOU NANDU ENERGY TECHNOLOGY Co Ltd
HANGZHOU NARADA BATTERY CO Ltd
Zhejiang Narada Power Source Co Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention provides a method for preparing a positive material of a high-power lithium ion battery. The positive material is LiNixCo1-x-yMnyO2 (0<=x, y<=1, and x+y<=1). The method comprises the following steps: choosing a 0.1-10mu m template ball body, performing emulsification dispersing on the template ball body, adding metal salt solution, then adding precipitator, enabling metal ions to evenly deposit on the surface of the template ball body under the effect of the precipitator, performing hot filtering on the template ball body with the metal ions deposited on the surface to obtain an organic-inorganic compound core shell structure material, and performing thermal treatment to obtain the hollow positive material by evenly mixing the organic-inorganic compound core shell structure material with the lithium salt, wherein the metal salt is metal salt of Ni, Co and Mn. The obtained ternary material has regular hollow spherical shape, is even in grain size and grain fineness distribution, can improve the absorbing/releasing capability on non-water electrolyte of active substances, effectively shortens embedding and de-embedding of the lithium ions, accordingly enhances the storage/transmission performance of the lithium ion battery, and provides effective support for large-current high-magnification charging and discharging, and the compounded ternary material can be applied to power battery materials.

Description

A kind of method for preparing the high power lithium ion cell positive electrode
Technical field
The present invention relates to technical field of lithium ion, be specifically related to a kind of high power lithium ion cell positive electrode LiNi xCo 1-x-yMn yO 2The preparation method of (0≤x, y≤1, x+y≤1).
Background technology
From the nineties in 20th century Sony successfully with LiCoO 2Push to after the commercialization market, the advantages such as lithium ion battery is high because of its specific capacity, have extended cycle life, security performance is good, environmentally friendly at home and abroad obtain extensively in mobile terminal devices such as various mobile phones, notebooks, but because high temperature and over-charging are poor, the toxicity of cobalt and costliness make it at high power electrokinetic cell field (electric bicycle in addition, electric motor car, communication base station equipment, weaponry and space flight and aviation equipment etc.) be restricted.Therefore, seek the alternative lithium ion anode material of a kind of high power and become the focus of expanding its application.
Nickel-cobalt lithium manganate material, i.e. ternary material LiNi xCo 1-x-yMn yO 2(0≤x, y≤1, x+y≤1) becomes one of hot topic that people competitively study.But ternary material is not LiCoO 2, LiNiO 2, Li 2MnO 4Three's simple fusion.On the one hand, ternary material draws LiCoO 2Good cycling stability, LiNiO 2Gram volume is high, Li 2MnO 4The advantage that safety is cheap has overcome LiCoO 2Poor, the LiNiO of overcharging resisting performance 2Preparation difficulty, Li 2MnO 4The inferior position of high temperature Mn dissolving; On the other hand, Co can reduce the stability that cation mixing erect-position strengthens layer structure, and Ni can provide the capacity of material, and Mn can reduce material cost, improves safety and stability.Ternary material utilizes Ni, Co, and Mn three's cooperative effect is brought into play the potential advantages of material to greatest extent.Yet ternary material and LiCoO 2Compare, its conductivity is on the low side to cause the performance of its heavy-current discharge and high rate capability to be subject to very big challenge.
Summary of the invention
Technical problem to be solved by this invention provides a kind of simple to operate, with low cost, preparation method that can obviously improve the high power type lithium ion positive electrode of large electric current power generation performance, this anode material nickel cobalt manganic acid lithium LiNi xCo 1-x-yMn yO 2(0≤x, y≤1, x+y≤1).For this reason, the present invention is by the following technical solutions: it may further comprise the steps:
Select the template spheroid of 0.1 ~ 10 μ m, again to its emulsion dispersion, then add first metal salt solution, add afterwards precipitation reagent, metal ion under the effect of precipitation reagent uniform settlement at the template spherome surface, the effects on surface sedimentation has the template spheroid heat filter of metal ion to obtain organic and inorganic complex nucleus shell structure material again, and after lithium salts evenly mixed, heat treatment obtained hollow positive electrode; Described slaine is Ni, Co, Mn slaine.
On the basis of adopting technique scheme, the present invention also can adopt following further technical scheme:
Described heat treatment is: the organic and inorganic complex nucleus shell structure material that filtration is obtained is warming up to 400 ~ 500 ℃ with the heating rate of 2 ~ 5 ℃/min under air atmosphere, be incubated 4 ~ 6h under this temperature.Heating rate with 2 ~ 10 ℃/min is warming up to 750 ~ 1000 ℃ again, is incubated 12 ~ 30h under this temperature, afterwards directly in air quenching to room temperature.
Ni, Co, Mn slaine used in this positive electrode preparation process are the nitrate of metal, sulfate, chlorate, one or more in the acetate.
Used template spheroid is polymethyl methacrylate (PMMA) microballoon in this positive electrode preparation process, polystyrene (PS), polyethylene (PE), a kind of in the polypropylene (PP).
In this positive electrode preparation process in the preparation process used precipitation reagent be urea, ammonium carbonate, one or more in the ammonium hydrogencarbonate.
Used lithium salts is LiF, Li in the described positive electrode preparation process 2CO 3, LiNO 3, LiOH, Li 2SO 4, CH 3Among COOLi, the LiCl one or more.
The chemical formula of described nickle cobalt lithium manganate can be LiNi 0.5Mn 0.5O 2, LiNi 1/3Co 1/3Mn 1/3O 2, LiNi 0.8Co 0.1Mn 0.1O 2, LiNi 0.4Co 0.2Mn 0.2O 2, LiNi 0.5Co 0.3Mn 0.2O 2, LiNi 0.7Co 0.15Mn 0.15O 2In one or more.
The particle diameter of described positive electrode can be from the nanometer to the micron level allotment, specifically be limited by the particle diameter of used hard template.
Template is to prepare in recent years to receive the important method of powder body.Can really realize to a certain extent the effective control to nano-micro structure.This method is less demanding to preparation condition, and is simple to operate.Can obtain by adjusting each parameter in the template preparation process that epigranular distributes, particle diameter is controlled, easily mix and hold manageable material.The template ratio juris is to utilize structural matrix as template, structural matrix such as Woelm Alumina, CNT (carbon nano-tube), porous glass, large space ion exchange resin, zeolite molecular sieve, high polymer, reversed micelle etc.Template by synthetic moderate size and structure is as theme, utilize physical chemistry method to wherein filling various metals, nonmetal or semi-conducting material, thereby obtain the object nano-structure array of required specific dimensions and function, such as self-assembled structures, solid nano wire or hollow nano-sphere, single component material or composite material and even wrapping biological material etc.
Because adopt technical scheme of the present invention, the present invention utilizes template auxiliary law synthesis of ternary material LiNi xCo 1-x-yMn yO 2(0≤x, y≤1, x+y≤1); The present invention compared with prior art has following advantage:
1), the well-regulated hollow ball pattern of gained ternary material tool, particle diameter even particle size distribution, overcome traditional solid reaction process and be difficult for obtaining to have the shortcoming of rule, uniform morphology material, be conducive to the further processing to material.Can regulate the particle diameter of ternary material hollow ball by changing rate of charge.
2), utilize the synthetic ternary material of template to have hollow structure, the structure of hollow ball-type pattern surface porosity porous helps fully contacting with wetting of material and electrolyte, energy enhanced activity material is to the suction storage/releasability of nonaqueous electrolyte, effectively shorten the embedding of lithium ion/take off embedding, thereby strengthened the storage/transmittability of lithium ion battery, for large electric current high power charging-discharging provides effective support, synthetic ternary material can be applicable to power battery material.
Description of drawings
Fig. 1 is the schematic diagram of the synthetic hollow ternary material of template of the present invention.
Hollow ball-type lithium ion anode material Electronic Speculum figure after Fig. 2 heat treatment.
Hollow ball-type lithium ion anode material X-ray diagram after Fig. 3 heat treatment.
Hollow ball-type lithium ion anode material is assembled into the electric high-multiplying power discharge cycle graph of button after Fig. 4 heat treatment
Embodiment
Embodiment 1:
Get 2mL polystyrene spheres (~ 2 μ m) in the 50mL beaker, drip 95% ethanol 5mL, deionized water 25mL, and ultrasonic 10min makes it disperse rear the taking-up, place in 80 ℃ of constant temperature water baths, with NiSO4, CoSO4, MnSO4 (mol ratio Ni:Co:Mn=1:1:1) solution B and the CO (NH after the dissolving 2) 2Solution A adds in the beaker successively, CO (NH 2) 2With the mol ratio of slaine be 6:1, mixing speed is 300rph.Heat filtering behind the reaction 24h, 80 ℃ of dryings of filter cake vacuum.With LiNO 3, be placed in the Muffle furnace than behind the mixing by metering, be warming up to 450 ℃ with the heating rate of 5 ℃/min, under this temperature, be incubated 5h.Heating rate with 10 ℃/min is warming up to 850 ℃ again, is incubated 24h under this temperature, afterwards directly in air quenching to room temperature.Obtain anodal ternary material LiNi 1/3Co 1/3Mn 1/3O 2
Embodiment 2
Get in 1mL acrylic sphere (100nm) and the 50mL beaker, drip 95% ethanol 5mL, deionized water 15mL, and ultrasonic 10min takes out after it is disperseed, and places in 80 ℃ of constant temperature water baths, with the NiCl after the dissolving 2, CoCl 2, MnCl 2(mol ratio Ni:Co:Mn=8:1:1) solution B and (NH 4) 2CO 3Solution A adds in the beaker successively, (NH 4) 2CO 3With the mol ratio of slaine be 4:1, mixing speed is 300rph.Heat filtering behind the reaction 24h, 80 ℃ of dryings of filter cake vacuum.With LiOH by metering than behind the mixing, be placed in the Muffle furnace, be warming up to 480 ℃ with the heating rate of 2 ℃/min, under this temperature, be incubated 4h.Heating rate with 5 ℃/min is warming up to 800 ℃ again, is incubated 28h under this temperature, afterwards directly in air quenching to room temperature.Obtain anodal ternary material LiNi 0.8Co 0.1Mn 0.1O 2
Embodiment 3
Get in 1mL polymethyl methacrylate ball (30nm) and the 50mL beaker, drip 95% ethanol 5mL, deionized water 15mL, and ultrasonic 10min takes out after it is disperseed, and places in 80 ℃ of constant temperature water baths, with the Ni (NO after the dissolving 3) 2, Co (NO 3) 2, Mn (NO 3) 2(mol ratio Ni:Co:Mn=4:2:2) solution B and NH 4HCO 3Solution A adds in the beaker successively, NH 4HCO 3With the mol ratio of slaine be 5:1, mixing speed is 300rph.Heat filtering behind the reaction 24h, 80 ℃ of dryings of filter cake vacuum.With LiOH by metering than behind the mixing, be placed in the Muffle furnace, be warming up to 480 ℃ with the heating rate of 2 ℃/min, under this temperature, be incubated 6h.Heating rate with 6 ℃/min is warming up to 860 ℃ again, is incubated 12h under this temperature, afterwards directly in air quenching to room temperature.Obtain anodal ternary material LiNi 0.4Co 0.2Mn 0.2O 2
Embodiment 4
Get in 3mL polyethylene ball (10 μ m) and the 50mL beaker, drip 95% ethanol 8mL, deionized water 15mL, and ultrasonic 10min takes out after it is disperseed, and places in 80 ℃ of constant temperature water baths, with the Ni (CH after the dissolving 3COO) 2, Co (CH 3COO) 2, Mn (CH 3COO) 2(mol ratio Ni:Co:Mn=5:3:2) solution B and sal volatile A add in the beaker successively, and the mol ratio of ammonium carbonate and slaine is 4:1, and mixing speed is 300rph.Heat filtering behind the reaction 24h, 80 ℃ of dryings of filter cake vacuum.With Li 2CO 3, be placed in the Muffle furnace than behind the mixing by metering, be warming up to 400 ℃ with the heating rate of 3 ℃/min, under this temperature, be incubated 6h.Heating rate with 8 ℃/min is warming up to 780 ℃ again, is incubated 30h under this temperature, afterwards directly in air quenching to room temperature.Obtain anodal ternary material LiNi 0.5Co 0.3Mn 0.2O 2
Embodiment 5
Get in 3mL acrylic sphere (10 μ m) and the 50mL beaker, drip 95% ethanol 8mL, deionized water 15mL, and ultrasonic 10min takes out after it is disperseed, and places in 80 ℃ of constant temperature water baths, with the Ni (CH after the dissolving 3COO) 2, Co (CH 3COO) 2, Mn (CH 3COO) 2(mol ratio Ni:Co:Mn=0.7:0.15:0.15) solution B and NH 4HCO 3Solution A adds in the beaker successively, NH 4HCO 3With the mol ratio of slaine be 4:1, mixing speed is 300rph.Heat filtering behind the reaction 24h, 80 ℃ of dryings of filter cake vacuum.With Li 2CO 3, be placed in the Muffle furnace than behind the mixing by metering, be warming up to 500 ℃ with the heating rate of 5 ℃/min, under this temperature, be incubated 4.5h.Heating rate with 4 ℃/min is warming up to 750 ℃ again, is incubated 28h under this temperature, afterwards directly in air quenching to room temperature.Obtain anodal ternary material LiNi 0.7Co 0.15Mn 0.15O 2
Embodiment 6
Get in 3mL acrylic sphere (5 μ m) and the 50mL beaker, drip 95% ethanol 8mL, deionized water 15mL, and ultrasonic 10min takes out after it is disperseed, and places in 80 ℃ of constant temperature water baths, with the Ni (CH after the dissolving 3COO) 2, Mn (CH 3COO) 2(mol ratio Ni:Mn=1: 1) solution B and CO (NH 2) 2Solution A adds in the beaker successively, CO (NH 2) 2With the mol ratio of slaine be 4:1, mixing speed is 300rph.Heat filtering behind the reaction 24h, 80 ℃ of dryings of filter cake vacuum.With LiCl by metering than behind the mixing, be placed in the Muffle furnace, be warming up to 450 ℃ with the heating rate of 5 ℃/min, under this temperature, be incubated 5h.Heating rate with 5 ℃/min is warming up to 750 ℃ again, is incubated 30h under this temperature, afterwards directly in air quenching to room temperature.Obtain anodal ternary material LiNi 0.5Mn 0.5O 2
With reference to Fig. 2,3,4, the product LiNi synthetic to the embodiment of the invention 1 1/3Co 1/3Mn 1/3O 2Make surface sweeping Electronic Speculum, X-ray diffraction, multiplying power Performance Analysis, its pattern, phase, performance are respectively shown in Fig. 2,3,4.It is made the positive electrode of lithium ion battery, make the button half-cell take the lithium sheet as negative pole, at 40mAcm -2Constant current is done charge-discharge test under the 2.5-4.4V voltage, and the result shows that initial discharge capacity is 138mAh/g, and discharge capacity is 122mAh/g after 50 circulations, proves that the product that the present invention synthesizes is fit to do anode material for lithium-ion batteries.

Claims (7)

1. method for preparing the high power lithium ion cell positive electrode, described positive electrode is LiNi xCo 1-x-yMn yO 2(0≤x, y≤1, x+y≤1); It is characterized in that it may further comprise the steps:
Select the template spheroid of 0.1 ~ 10 μ m, again to its emulsion dispersion, then add first metal salt solution, add afterwards precipitation reagent, metal ion under the effect of precipitation reagent uniform settlement at the template spherome surface, the effects on surface sedimentation has the template spheroid heat filter of metal ion to obtain organic and inorganic complex nucleus shell structure material again, and after lithium salts evenly mixed, heat treatment obtained hollow positive electrode; Described slaine is Ni, Co, Mn slaine.
2. method as claimed in claim 1 is characterized in that, heat treatment method is: the organic and inorganic complex nucleus shell structure material that filtration is obtained is warming up to 400 ~ 500 ℃ with the heating rate of 2 ~ 5 ℃/min under air atmosphere, be incubated 4 ~ 6h under this temperature.Heating rate with 2 ~ 10 ℃/min is warming up to 750 ~ 1000 ℃ again, is incubated 12 ~ 30h under this temperature, afterwards directly in air quenching to room temperature.
3. method as claimed in claim 1 is characterized in that, Ni, Co, Mn slaine used in the preparation process are the nitrate of metal, sulfate, chlorate, one or more in the acetate.
4. method as claimed in claim 1 is characterized in that, used template spheroid is polymethyl methacrylate (PMMA) microballoon in the preparation process, polystyrene (PS), polyethylene (PE), a kind of in the polypropylene (PP).
5. method as claimed in claim 1 is characterized in that, in the preparation process in the preparation process used precipitation reagent be urea, ammonium carbonate, one or more in the ammonium hydrogencarbonate.
6. method as claimed in claim 1 is characterized in that, used lithium salts is LiF, Li in the preparation process 2CO 3, LiNO 3, LiOH, Li 2SO 4, CH 3Among COOLi, the LiCl one or more.
7. method as claimed in claim 1 is characterized in that, the chemical formula of described nickle cobalt lithium manganate is: LiNi 0.5Mn 0.5O 2, LiNi 1/3Co 1/3Mn 1/3O 2, LiNi 0.8Co 0.1Mn 0.1O 2, LiNi 0.4Co 0.2Mn 0.2O 2, LiNi 0.5Co 0.3Mn 0.2O 2, LiNi 0.7Co 0.15Mn 0.15O 2In one or more.
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Cited By (14)

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CN103441239A (en) * 2013-07-22 2013-12-11 彩虹集团公司 Synthetic method for nanoscale ternary cathode material
CN103531763A (en) * 2013-10-24 2014-01-22 广东邦普循环科技股份有限公司 Preparation method of nickel cobalt lithium manganate
CN103779612A (en) * 2013-12-19 2014-05-07 宁波维科电池股份有限公司 Preparation method of flexibly packaged lithium ion power battery
CN104241630A (en) * 2014-07-10 2014-12-24 奇瑞汽车股份有限公司 Lithium nickel cobalt manganate hollow sphere as well as preparation method and application thereof
CN104362335A (en) * 2014-11-29 2015-02-18 冀明 Preparation method of lithium nickel cobalt manganese oxide positive electrode material
CN104766998A (en) * 2015-03-24 2015-07-08 江苏乐能电池股份有限公司 A preparing method of a high-power high-energy density lithium ion battery
CN104779374A (en) * 2015-04-23 2015-07-15 天津巴莫科技股份有限公司 Preparation method of high-performance hollow manganese lithium phosphate for lithium ion powder battery
CN107445214A (en) * 2017-09-05 2017-12-08 中南大学 A kind of lithium ion battery nickel-cobalt-manganternary ternary anode material and preparation method thereof
CN109052490A (en) * 2018-07-09 2018-12-21 华中科技大学 A kind of ternary cathode material of lithium ion battery and preparation method thereof
CN109346720A (en) * 2018-12-06 2019-02-15 河南科隆新能源股份有限公司 A kind of preparation method of high multiplying power lithium ion tertiary cathode material
CN109835956A (en) * 2019-01-11 2019-06-04 天津巴莫科技股份有限公司 A kind of preparation method and applications of anode material for lithium-ion batteries
CN109860540A (en) * 2018-12-20 2019-06-07 天津巴莫科技股份有限公司 A kind of high performance nickel cobalt lithium aluminate cathode material and preparation method thereof
CN110299535A (en) * 2018-03-23 2019-10-01 比亚迪股份有限公司 A kind of ternary material precursor and preparation method thereof, ternary material and battery
CN115057488A (en) * 2022-07-12 2022-09-16 合肥国轩高科动力能源有限公司 Lithium ion battery positive electrode material with special morphology and preparation method and application thereof

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CN103441239A (en) * 2013-07-22 2013-12-11 彩虹集团公司 Synthetic method for nanoscale ternary cathode material
CN103531763B (en) * 2013-10-24 2015-12-02 广东邦普循环科技有限公司 A kind of method preparing nickle cobalt lithium manganate
CN103531763A (en) * 2013-10-24 2014-01-22 广东邦普循环科技股份有限公司 Preparation method of nickel cobalt lithium manganate
CN103779612A (en) * 2013-12-19 2014-05-07 宁波维科电池股份有限公司 Preparation method of flexibly packaged lithium ion power battery
CN104241630A (en) * 2014-07-10 2014-12-24 奇瑞汽车股份有限公司 Lithium nickel cobalt manganate hollow sphere as well as preparation method and application thereof
CN104241630B (en) * 2014-07-10 2017-02-22 奇瑞汽车股份有限公司 Lithium nickel cobalt manganate hollow sphere as well as preparation method and application thereof
CN104362335A (en) * 2014-11-29 2015-02-18 冀明 Preparation method of lithium nickel cobalt manganese oxide positive electrode material
CN104766998A (en) * 2015-03-24 2015-07-08 江苏乐能电池股份有限公司 A preparing method of a high-power high-energy density lithium ion battery
CN104779374A (en) * 2015-04-23 2015-07-15 天津巴莫科技股份有限公司 Preparation method of high-performance hollow manganese lithium phosphate for lithium ion powder battery
CN107445214A (en) * 2017-09-05 2017-12-08 中南大学 A kind of lithium ion battery nickel-cobalt-manganternary ternary anode material and preparation method thereof
CN107445214B (en) * 2017-09-05 2019-06-04 中南大学 A kind of lithium ion battery nickel-cobalt-manganternary ternary anode material and preparation method thereof
CN110299535A (en) * 2018-03-23 2019-10-01 比亚迪股份有限公司 A kind of ternary material precursor and preparation method thereof, ternary material and battery
CN110299535B (en) * 2018-03-23 2022-09-09 比亚迪股份有限公司 Ternary material precursor, preparation method thereof, ternary material and battery
CN109052490A (en) * 2018-07-09 2018-12-21 华中科技大学 A kind of ternary cathode material of lithium ion battery and preparation method thereof
CN109052490B (en) * 2018-07-09 2019-11-22 华中科技大学 A kind of ternary cathode material of lithium ion battery and preparation method thereof
CN109346720A (en) * 2018-12-06 2019-02-15 河南科隆新能源股份有限公司 A kind of preparation method of high multiplying power lithium ion tertiary cathode material
CN109860540A (en) * 2018-12-20 2019-06-07 天津巴莫科技股份有限公司 A kind of high performance nickel cobalt lithium aluminate cathode material and preparation method thereof
CN109835956A (en) * 2019-01-11 2019-06-04 天津巴莫科技股份有限公司 A kind of preparation method and applications of anode material for lithium-ion batteries
CN115057488A (en) * 2022-07-12 2022-09-16 合肥国轩高科动力能源有限公司 Lithium ion battery positive electrode material with special morphology and preparation method and application thereof

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