CN104716315A - Preparation method of lithium ion batteries cathode material solid solution with core-shell structure - Google Patents

Preparation method of lithium ion batteries cathode material solid solution with core-shell structure Download PDF

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CN104716315A
CN104716315A CN201310679957.9A CN201310679957A CN104716315A CN 104716315 A CN104716315 A CN 104716315A CN 201310679957 A CN201310679957 A CN 201310679957A CN 104716315 A CN104716315 A CN 104716315A
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solution
preparation
solid solution
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孙琦
李岩
刘燕杰
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QINGDAO QIANYUN HIGH-TECH NEW MATERIAL Co Ltd
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QINGDAO QIANYUN HIGH-TECH NEW MATERIAL 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
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention relates to a preparation method of a lithium ion batteries cathode material solid solution with a core-shell structure. The solid solution is prepared by a two-step coprecipitation method, a molecular formula of the core-shell structure is Li1+y[(Mn1/3Ni1/3Co1/3)x(Ni1/4Mn3/4)1-x]1-yO2. The method comprises the following steps: spherical [Mn1/3Ni1/3Co1/3]CO3 is synthesized in a stirring reactor through the coprecipitation method, then nickel salt and manganese salt are placed in a reactor according to mol ratio of 1: 3, then a [Mn1/3Ni1/3Co1/3]CO3 precursor with the core-shell structure is obtained through a secondary coprecipitation method, and the precursor and the lithium salt are mixed for calcination to obtain the lithium ion batteries cathode material solid solution with the core-shell structure. The obtained product has excellent electrochemistry property, the preparation method is simple, and is suitable for large scale industrial production.

Description

A kind of preparation method of nucleocapsid structure lithium ion battery positive electrode solid solution
Technical field
The present invention relates to novel energy resource material technology field, be specifically related to a kind of preparation method of nucleocapsid structure lithium ion battery positive electrode solid solution.
Background technology
Along with the progress of science and technology, the fields such as electronic product, electric automobile, Medical Devices and space flight and aviation are improved day by day to the requirement of energy storage device, and energy density is high, volume is little, the lithium ion battery that has extended cycle life is used widely.Wherein, traditional positive electrode LiCoO 2capacity is low, cost is high; And LiNiO 2synthesis condition is harsh, and invertibity is poor; The LiFePO of relative low price 4ionic conductivity is poor, and actual discharge specific capacity only has 160 mAh/g.These anode material for lithium-ion batteries are difficult to meet high power capacity, high-energy-density electronic product
Demand.Lithium-rich anode material Li in recent years 1+x[M] 1-xo 2(M=Co, Ni, Mn ...) comparatively LiCoO 2having height ratio capacity (200 ~ 300 mAh/g) and lower price and receive increasing concern, is positive electrode current commercialization main product LiCoO 2good substitute.
At present, what paid close attention to by people is the layed solid-solution product containing Co, Li 1+x(Mn 1/3ni 1/3co 1/3) 1-xo 2than Li (Mn 1/3ni 1/3co 1/3) O 2show better high rate performance and thermal stability, but at voltage higher than having an irreversible capacity loss close to 200mAh/g during 4.5V, and this material also also exists the problem of cyclical stability.Main cause is in the process of discharge and recharge, Co dissolving under high voltages causes collapsing of material monolithic structure, although many researchers solve this problem by surface modification, but the insulating properties due to coating can cause the increase of battery impedance, and this thin coating easily comes off in subsequent processes, therefore can not suitability for industrialized production.Another kind of rich lithium stratified material Li 1+x(Mn 3/4ni 1/4) 1-xo 2, because its non-toxic, high power capacity, stability and good cyclicity are studied widely.But due to insulation phase Li 2mnO 3existence, the poorly conductive of this material, thus cause its high rate performance bad, limits its application on electric automobile.
Therefore, bi-material is combined, utilize the cooperative effect between them, the electrode material of high magnification and high cyclical stability can be obtained.
Summary of the invention
Object of the present invention is just being to provide the preparation method of the nucleocapsid structure solid solution of a kind of high magnification and high cyclical stability electrode material.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the preparation method of the anode material of lithium battery solid solution of described a kind of nucleocapsid structure is, taking required Mn salt, Ni salt and Co salt by the stoichiometric proportion of 1:1:1 is dissolved in deionized water, be made into certain density metal salt solution, ie in solution 1; The sodium carbonate liquor of preparation and above-mentioned total metal ion same concentrations, adding ammoniacal liquor is complexing agent, and ammonia concn is 0.1 – 0.4 mol/L; With peristaltic pump, solution 1 and sodium carbonate liquor are input in reaction flask continuously, controlling flow is 5ml/min – 20ml/min, within the scope of bath temperature 53 – 58 ° of C of reactor, slurries pH controls in 6.5 – 8.5 scopes, and mixing speed controls at 500 – 650 rmp; After reacting completely, the mol ratio of nickel salt and manganese salt stoichiometrically 1:3 is made into certain density solution 2; The sodium carbonate liquor 2 of preparation and solution 2 same concentrations, adding ammoniacal liquor is complexing agent, and ammonia concn is 0.1 – 0.4 mol/L; Solution 2 and sodium carbonate liquor 2 are input in reaction flask by peristaltic pump continuously, control flow is 5ml/min-20ml/min, within the scope of bath temperature 53 – 58 ° of C of reactor, slurries pH controls in 6.5 – 8.5 scopes, and mixing speed controls at 500 – 650 rmp; After having reacted, precipitation is carried out centrifugation, with distilled water repeatedly wash removing survivor ion after 50-100 ° of C drying, obtain presoma for subsequent use; By presoma and a certain amount of Li 2cO 3or LiOH mixing is ground into powder evenly carry out preroast in air atmosphere.
Above-mentioned slaine is nitrate, sulfate or acetate.
Above-mentioned solution 1 and the total concentration of solution 2 are 0.5 – 3 mol/L.
The temperature of above-mentioned preroast controls at 400 –, 600 ° of C, roasting time 3-6 h, and the temperature of rear roasting controls at 800 –, 1000 ° of C, roasting time 10 – 25h, and heating rate is 3-10 ° of C/min.
Advantage of the present invention: the present invention adopts two step coprecipitations to prepare solid solution cathode material, and obtained material is the micron ball of nucleocapsid structure, improves the tap density of material, thus be conducive to improving material volume specific energy.With Li 1+x(Mn 1/3ni 1/3co 1/3) 1-xo 2for core, with Li 1+x(Mn 3/4ni 1/4) 1-xo 2for shell, utilize the core of this spheroidal material and the synergistic effect of shell, the material obtaining a kind of high-energy-density, high rate capability and good cyclical stability can be expected to.
Accompanying drawing explanation
Fig. 1 is Li of the present invention 1.2[(Mn 1/3ni 1/3co 1/3) 0.5(Ni 1/4mn 3/4) 0.5] 0.8o 2low power SEM figure;
Fig. 2 is Li of the present invention 1.2[(Mn 1/3ni 1/3co 1/3) 0.5(Ni 1/4mn 3/4) 0.5] 0.8o 2high power SEM figure;
Fig. 3 is Li of the present invention 1.2[(Mn 1/3ni 1/3co 1/3) 0.5(Ni 1/4mn 3/4) 0.5] 0.8o 2and Li 1.2(Ni 1/4mn 3/4) 0.8o 2circulation compare, (a) Li 1.2[(Mn 1/3ni 1/3co 1/3) 0.5(Ni 1/4mn 3/4) 0.5] 0.8o 2(b) Li 1.2(Ni 1/4mn 3/4) 0.8o 2.
Embodiment
Embodiment 1
Solid solution Li 1.2[(Mn 1/3ni 1/3co 1/3) 0.5(Ni 1/4mn 3/4) 0.5] 0.8o 2preparation process
(1) required MnSO is taken by the stoichiometric proportion of 1:1:1 4, NiSO 4salt and CoSO 4salt is dissolved in deionized water, is made into the solution that 300ml concentration is 1.5mol/L.
(2) prepare the sodium carbonate liquor of 300ml and above-mentioned total metal ion same concentrations, adding ammoniacal liquor is complexing agent, and ammonia concn is 0.2 mol/L.
(3) metal salt solution and sodium carbonate liquor are input to continuously in reaction flask with peristaltic pump, control flow is 5ml/min, bath temperature 55 ° of C scopes of reactor, and it is 8 that slurries pH controls, and mixing speed controls at 600 rmp.
(4) after stirring reaction 3h, by NiSO 4with MnSO 4stoichiometrically the mol ratio of 1:3 is made into the solution that 300ml concentration is 1.5mol/L.
(5) prepare the sodium carbonate liquor of 300ml and the total metal ion same concentrations of (4) step, adding ammoniacal liquor is complexing agent, and ammonia concn is 0.2 mol/L.
(6) metal salt solution of (4) step and the sodium carbonate liquor of (5) step are input in reaction flask by peristaltic pump continuously, control flow is 5ml/min, bath temperature 55 ° of C scopes of reactor, it is 8 that slurries pH controls, and mixing speed controls at 600 rmp.
(7) after having reacted, precipitation is carried out centrifugation, with distilled water repeatedly wash removing survivor ion after 100 ° of C dryings, obtain presoma for subsequent use.
(8) be that 0.8:0.6 is by presoma and Li in molar ratio 2cO 3roasting in air atmosphere is evenly ground in mixing into powder.First preroast 5 h, then roasting 10h under 900 ° of C under 500 ° of C, heating rate is 5 ° of C/min.
Embodiment 2
Solid solution Li 1.1[(Mn 1/3ni 1/3co 1/3) 0.5(Ni 1/4mn 3/4) 0.5] 0.9o 2preparation process
(1) – (7) step is with embodiment 3
(8) be that 1.1:0.45 is by presoma and Li in molar ratio 2cO 3roasting in air atmosphere is evenly ground in mixing into powder.First preroast 5 h, then roasting 10h under 800 –, 1000 ° of C under 400 –, 600 ° of C, heating rate is 5 ° of C/min.
 
Embodiment 3
Solid solution Li 1.2[(Mn 1/3ni 1/3co 1/3) 0.7(Ni 1/4mn 3/4) 0.3] 0.8o 2preparation process
(1) required Mn (NO is taken by the stoichiometric proportion of 1:1:1 3) 2, Ni (NO 3) 2salt and Co (NO 3) 2salt is dissolved in deionized water, is made into the solution that 400ml concentration is 1.4mol/L.
(2) prepare the sodium carbonate liquor of 400ml and above-mentioned total metal ion same concentrations, adding ammoniacal liquor is complexing agent, and ammonia concn is 0.2 mol/L.
(3) metal salt solution and sodium carbonate liquor are input to continuously in reaction flask with peristaltic pump, control flow is 5ml/min, bath temperature 55 ° of C scopes of reactor, and it is 8 that slurries pH controls, and mixing speed controls at 600 rmp.
(4) after stirring reaction 3h, by Ni (NO 3) 2with Mn (NO 3) 2stoichiometrically the mol ratio of 1:3 is made into the solution that 200ml concentration is 1.2mol/L.
(5) prepare the sodium carbonate liquor of 200ml and the total metal ion same concentrations of (4) step, adding ammoniacal liquor is complexing agent, and ammonia concn is 0.2 mol/L.
(6) metal salt solution of (4) step and the sodium carbonate liquor of (5) step are input in reaction flask by peristaltic pump continuously, control flow is 5ml/min, bath temperature 55 ° of C scopes of reactor, it is 8 that slurries pH controls, and mixing speed controls at 600 rmp.
(7) after having reacted, precipitation is carried out centrifugation, with distilled water repeatedly wash removing survivor ion after 100 ° of C dryings, obtain presoma for subsequent use.
(8) be that 0.8:0.6 is by presoma and Li in molar ratio 2cO 3roasting in air atmosphere is evenly ground in mixing into powder.First preroast 5 h, then roasting 10h under 900 ° of C under 500 ° of C, heating rate is 5 ° of C/min.
Embodiment 4
Comparative example Li 1.2(Ni 1/4mn 3/4) 0.8o 2preparation process
(1) by NiSO 4with MnSO 4stoichiometrically the mol ratio of 1:3 is made into the solution that 300ml concentration is 1.5mol/L.
(2) prepare the sodium carbonate liquor of 300ml and the total metal ion same concentrations of (1) step, adding ammoniacal liquor is complexing agent, and ammonia concn is 0.2 mol/L.
(3) metal salt solution of (1) step and the sodium carbonate liquor of (2) step are input in reaction flask by peristaltic pump continuously, control flow is 5ml/min, bath temperature 55 ° of C scopes of reactor, it is 8 that slurries pH controls, and mixing speed controls at 600 rmp.
(4) after having reacted, precipitation is carried out centrifugation, with distilled water repeatedly wash removing survivor ion after 100 ° of C dryings, obtain presoma for subsequent use.
(5) be that 0.8:0.6 is by presoma and Li in molar ratio 2cO 3roasting in air atmosphere is evenly ground in mixing into powder.First preroast 5 h, then roasting 10h under 900 ° of C under 500 ° of C, heating rate is 5 ° of C/min.
Fig. 1 is Li of the present invention 1.2[(Mn 1/3ni 1/3co 1/3) 0.5(Ni 1/4mn 3/4) 0.5] 0.8o 2low power SEM figure.
From figure, we can find out that this solid solution is for spherical uniformly, and size is 15 – about 20 μm.Fig. 2 is Li of the present invention 1.2[(Mn 1/3ni 1/3co 1/3) 0.5(Ni 1/4mn 3/4) 0.5] 0.8o 2high power SEM figure.From figure, we significantly can observe this spherical material is nucleocapsid structure.
Fig. 3 is Li of the present invention 1.2[(Mn 1/3ni 1/3co 1/3) 0.5(Ni 1/4mn 3/4) 0.5] 0.8o 2and Li 1.2(Ni 1/4mn 3/4) 0.8o 2circulation compare, as can be seen from figure we, Li 1.2(Mn 1/3ni 1/3co 1/3) 0.8o 2significantly can improve Li 1.2(Ni 1/4mn 3/4) 0.8o 2high rate capability, and multiplying power is higher, and the effect of improvement is more obvious.
The present invention adopts two step coprecipitations to prepare solid solution cathode material, and obtained material is the micron ball of nucleocapsid structure, improves the tap density of material, thus is conducive to improving material volume specific energy.With Li 1+x(Mn 1/3ni 1/3co 1/3) 1-xo 2for core, with Li 1+x(Mn 3/4ni 1/4) 1-xo 2for shell, utilize the core of this spheroidal material and the synergistic effect of shell, the material obtaining a kind of high-energy-density, high rate capability and good cyclical stability can be expected to.
Certainly, above-mentioned explanation is not limitation of the present invention, and the present invention is also not limited to above-mentioned citing; those skilled in the art; in essential scope of the present invention, the change made, remodeling, interpolation or replacement, all should belong to protection scope of the present invention.

Claims (4)

1. the preparation method of the anode material of lithium battery solid solution of a nucleocapsid structure, it is characterized in that: the preparation method of the anode material of lithium battery solid solution of described a kind of nucleocapsid structure is, taking required Mn salt, Ni salt and Co salt by the stoichiometric proportion of 1:1:1 is dissolved in deionized water, be made into certain density metal salt solution, ie in solution 1; The sodium carbonate liquor of preparation and above-mentioned total metal ion same concentrations, adding ammoniacal liquor is complexing agent, and ammonia concn is 0.1 – 0.4 mol/L; With peristaltic pump, solution 1 and sodium carbonate liquor are input in reaction flask continuously, controlling flow is 5ml/min – 20ml/min, within the scope of bath temperature 53 – 58 ° of C of reactor, slurries pH controls in 6.5 – 8.5 scopes, and mixing speed controls at 500 – 650 rmp; After reacting completely, the mol ratio of nickel salt and manganese salt stoichiometrically 1:3 is made into certain density solution 2; The sodium carbonate liquor 2 of preparation and solution 2 same concentrations, adding ammoniacal liquor is complexing agent, and ammonia concn is 0.1 – 0.4 mol/L; Solution 2 and sodium carbonate liquor 2 are input in reaction flask by peristaltic pump continuously, control flow is 5ml/min-20ml/min, within the scope of bath temperature 53 – 58 ° of C of reactor, slurries pH controls in 6.5 – 8.5 scopes, and mixing speed controls at 500 – 650 rmp; After having reacted, precipitation is carried out centrifugation, with distilled water repeatedly wash removing survivor ion after 50-100 ° of C drying, obtain presoma for subsequent use; By presoma and a certain amount of Li 2cO 3or LiOH mixing is ground into powder evenly carry out preroast in air atmosphere.
2. the preparation method of the anode material of lithium battery solid solution of a kind of nucleocapsid structure according to claim 1, is characterized in that: described slaine is nitrate, sulfate or acetate.
3. the preparation method of the anode material of lithium battery solid solution of a kind of nucleocapsid structure according to claim 1, is characterized in that: the total concentration of the solution 2 of described solution 1 is 0.5 – 3 mol/L.
4. the preparation method of the anode material of lithium battery solid solution of a kind of nucleocapsid structure according to claim 1, it is characterized in that: the temperature of described preroast controls at 400 –, 600 ° of C, roasting time 3-6 h, the temperature of rear roasting controls at 800 –, 1000 ° of C, roasting time 10 – 25h, heating rate is 3-10 ° of C/min.
CN201310679957.9A 2013-12-16 2013-12-16 Preparation method of lithium ion batteries cathode material solid solution with core-shell structure Pending CN104716315A (en)

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Cited By (3)

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CN109755549A (en) * 2019-03-11 2019-05-14 清远佳致新材料研究院有限公司 Nickel-base anode material and preparation method thereof, lithium ion cell positive, lithium ion battery and application
CN112531155A (en) * 2019-09-17 2021-03-19 湖南杉杉新能源有限公司 Preparation method of positive electrode material precursor and preparation method of positive electrode material
WO2021103879A1 (en) * 2019-11-29 2021-06-03 蜂巢能源科技有限公司 Carbonate precursor having high-nickel and low-cobalt sandwich structure, preparation method therefor and application thereof

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Application publication date: 20150617