CN106229477A - Positive electrode active materials, preparation method and application - Google Patents
Positive electrode active materials, preparation method and application Download PDFInfo
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- CN106229477A CN106229477A CN201610663573.1A CN201610663573A CN106229477A CN 106229477 A CN106229477 A CN 106229477A CN 201610663573 A CN201610663573 A CN 201610663573A CN 106229477 A CN106229477 A CN 106229477A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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 invention discloses a kind of positive electrode active materials, preparation method and application, belong to technical field of lithium ion.In the present invention, positive electrode active materials is by the LiNi of mass percent 60%～85%:15%～40%0.82Co0.15Al0.03O2And LiNi0.34Co0.32Mn0.34O2Composition, the D50 of the two is respectively 10～15 μm and 1～6 μm.Poor owing to there is particle diameter, both active materials can be homogenously mixed together, and on the one hand keeps the high specific discharge capacity of nickel cobalt lithium aluminate, on the other hand gives full play to high safety performance and the cycle performance of nickle cobalt lithium manganate.Compare the lithium ion battery of positive electrode in single use nickel cobalt lithium aluminate or nickel-cobalt lithium manganate cathode material and comparative example, use the lithium ion battery that in the present invention prepared by positive electrode to have higher discharge capacity and good high temperature cyclic performance, excellent cryogenic property and security performance.
Description
Technical field
The present invention relates to a kind of positive electrode active materials, also relate to the preparation method and application of this positive electrode active materials,
Belong to technical field of lithium ion.
Background technology
Along with the continuous quickening of electric automobile spreading speed, the course continuation mileage that customer demand is longer, therefore to power current
The energy density in pond proposes new challenge.And solve the prominent of the battery material technology that it is critical only that of electrokinetic cell energy density
Broken." energy-conservation and new-energy automobile industrial development planning (2012-2020) " issued by the State Council proposes target: moved to 2015
The energy density of power battery module reaches 150Wh/Kg (being converted to cell, its energy density is 170～190Wh/Kg), extremely
The energy density of the year two thousand twenty power battery module reaches 300Wh/Kg, and (energy density of corresponding cell is at least up to 330Wh/
Kg)。
At present, domestic most electrokinetic cell manufacturing enterprise uses LiFePO4 as positive electrode.It is known that iron phosphate
Lithium positive pole can be greatly promoted the security performance that battery is overall, and battery life is longer compared with other types battery.But, LiFePO4
The energy density of battery at most can only achieve 140～150Wh/Kg, less than 150Wh/Kg and the Future targets of national requirements
300Wh/Kg, therefore to have the positive electrode of high-energy-density imperative in exploitation.
In recent years, along with tesla's electric automobile persistently selling well in international power vehicle field, its matching used day
This Panasonic 18650 battery also gets more and more people's extensive concerning.The positive electrode that this battery uses is nickel cobalt aluminum (NCA) ternary material
Material, monomer mass energy density is up to 230Wh/Kg, far above at present with the lithium ion battery of type.But, NCA positive electrode
The high-energy-density problem of simultaneously also bringing battery high security risk.Therefore, the most effectively solve its safety problem to become
The key factor of restriction NCA large-scale promotion application.
The patent of invention of publication No. CN104218234A discloses a kind of lithium ion battery with high cycle performance and is combined
Positive electrode, by LiNi1-m-nComAlnO2、LiNiaCo1-a-bMnbO2After mixing, sintering or surface process and prepare, wherein 0.1 ＜ m
＜ 0.3,0.01 ＜ n ＜ 0.2,0 ＜ 1-m-n ＜ 1,0 ＜ a ＜ 1,0 ＜ b ＜ 1,0 ＜ 1-a-b ＜ 1, nickel cobalt lithium aluminate accounts for and is just being combined
The 10～90% of pole quality of materials, and the D50 of bi-material is 5～20 μm.Compare nickle cobalt lithium manganate, this composite positive pole
Specific capacity be greatly improved, and heat stability, security performance and cycle performance are substantially better than nickel cobalt lithium aluminate.But, composite wood
Material overall performance still has room for promotion.
Summary of the invention
It is an object of the invention to provide a kind of positive electrode active materials with high safety performance and high temperature cyclic performance.
Meanwhile, the present invention also provides for the preparation method of a kind of positive electrode active materials.
Finally, the present invention reoffers the application of a kind of above-mentioned positive electrode active materials.
In order to realize object above, the technical solution adopted in the present invention is:
Positive electrode active materials, by nickel cobalt lithium aluminate LiNi0.82Co0.15Al0.03O2And nickle cobalt lithium manganate
LiNi0.34Co0.32Mn0.34O2Composition, be calculated in mass percent, nickel cobalt lithium aluminate 60%～85%, nickle cobalt lithium manganate 15%～
40%.
The D50 of described nickel cobalt lithium aluminate is 10～15 μm, and the D50 of nickle cobalt lithium manganate is 1～6 μm.
Preferably, the D50 of nickel cobalt lithium aluminate is 13 μm, and the D50 of nickle cobalt lithium manganate is 4 μm.
The preparation of positive electrode active materials can use the method disclosed in the patent documentation of publication No. CN104218234A, it is possible to
Use following steps: accurately take nickel cobalt lithium aluminate and nickle cobalt lithium manganate, ball milling after mixing according to mass percent, to obtain final product.
The rotating speed of described ball milling is 80～120rpm, Ball-milling Time 1～2h.
Preferably, ball milling 1.5h under rotating speed 100rpm.
Positive electrode active materials is at positive electrode and prepares the application in lithium ion battery.
Concrete, positive electrode is made up of positive electrode active materials, conductive agent and binding agent, is calculated in mass percent, positive pole
Active material 90%～95%, conductive agent 1%～6%, binding agent 1%～6%.
Described conductive agent is white carbon black or acetylene black.
Described binding agent is Kynoar.
Concrete, lithium ion battery uses above-mentioned positive electrode active materials, and negative active core-shell material uses Delanium or natural
Graphite, barrier film uses polyethylene ceramic diaphragm.Positive pole, barrier film, negative pole stack and use laminated structure or takeup type knot successively
Structure constitutes core.Battery container can use aluminum hull, box hat or polymer packaging film (commercially available).
For making positive electrode mix homogeneously, and facilitate follow-up painting work, typically add a certain amount of in positive electrode
Solvent prepare anode sizing agent, solvent can use N-Methyl pyrrolidone, deionized water etc..In pole piece dry run, solvent
It is close to and volatilizees completely, the most do not constitute the component of positive electrode.
Beneficial effects of the present invention:
In the present invention, positive electrode active materials is by the nickel cobalt lithium aluminate of mass percent 70%～85%:15%～30%
LiNi0.82Co0.15Al0.03O2With nickle cobalt lithium manganate LiNi0.34Co0.32Mn0.34O2Composition, the D50 of the two be respectively 10～15 μm and
1～6 μm.Poor owing to there is particle diameter, both active materials can be homogenously mixed together, and on the one hand keeps the height of nickel cobalt lithium aluminate
Specific discharge capacity, on the other hand gives full play to high safety performance and the cycle performance of nickle cobalt lithium manganate.Compare single use nickel cobalt
In lithium aluminate or nickel-cobalt lithium manganate cathode material and comparative example, the lithium ion battery of positive electrode, uses positive pole material in the present invention
The lithium ion battery of material preparation has higher discharge capacity and good high temperature cyclic performance, excellent cryogenic property and peace
Full performance, its energy density reaches more than 220Wh/Kg, and 25 DEG C of circulations reach more than 2000 times.
In the present invention, the preparation technology of positive electrode active materials is simple, easy and simple to handle, is suitable to large-scale industrial and produces and application.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of positive electrode in test example 1；
Fig. 2 be in test example 2 positive electrode initial charge completely after differential thermal analysis curve；
Fig. 3 is the first charge-discharge curve of positive electrode in test example 3；
Fig. 4 is the room temperature cyclic curve of positive electrode in test example 4.
Detailed description of the invention
The present invention is only described in further detail by following embodiment, but does not constitute any limitation of the invention.
Embodiment 1
Positive electrode active materials, by nickel cobalt lithium aluminate LiNi0.82Co0.15Al0.03O2And nickle cobalt lithium manganate
LiNi0.34Co0.32Mn0.34O2Composition, is calculated in mass percent, nickel cobalt lithium aluminate 78%, nickle cobalt lithium manganate 22%.Nickel cobalt aluminic acid
The crystal grain of lithium is spherical, and D50 is 13 μm, and the crystal grain of nickle cobalt lithium manganate is that class is spherical, and D50 is 4 μm.
The preparation process of positive electrode active materials is as follows: accurately take nickel cobalt lithium aluminate and nickel cobalt mangaic acid according to mass percent
Lithium, puts into after mixing in ball grinder, and under rotating speed 100rpm, ball milling 1.5h, to obtain final product.
Positive electrode, is made up of above-mentioned positive electrode active materials, white carbon black (conductive agent) and Kynoar (binding agent), with matter
Amount percent meter, positive electrode active materials 94%, white carbon black 3%, Kynoar 3%.
Lithium ion battery, including positive pole, negative pole, barrier film, electrolyte and housing, positive pole uses above-mentioned positive electrode, negative pole
Material is mass percent than for the native graphite of 95%:1.4%:1.6%:2%, sodium carboxymethyl cellulose (CMC), butylbenzene rubber
Glue (SBR) and white carbon black composition, barrier film uses polyethylene ceramic diaphragm, and electrolyte uses nickelic positive electrode special electrolysis liquid (to purchase
It is bestowed by heaven from Guangzhou), housing is aluminum hull.After positive pole, barrier film, negative pole stack successively, constituted core with laminated structure, core is put
In aluminum hull, pour into electrolyte post package, obtain battery.
Embodiment 2
Positive electrode active materials, by nickel cobalt lithium aluminate LiNi0.82Co0.15Al0.03O2And nickle cobalt lithium manganate
LiNi0.34Co0.32Mn0.34O2Composition, is calculated in mass percent, nickel cobalt lithium aluminate 70%, nickle cobalt lithium manganate 30%.Nickel cobalt aluminic acid
The crystal grain of lithium is spherical, and D50 is 10 μm, and the crystal grain of nickle cobalt lithium manganate is that class is spherical, and D50 is 1 μm.
The preparation process of positive electrode active materials is as follows: accurately take nickel cobalt lithium aluminate and nickel cobalt mangaic acid according to mass percent
Lithium, puts into after mixing in ball grinder, and under rotating speed 120rpm, ball milling 1h, to obtain final product.
Positive electrode, by above-mentioned positive electrode active materials, acetylene black and Kynoar composition, is calculated in mass percent, just
Pole active material 90%, acetylene black 4%, Kynoar 6%.
Lithium ion battery, positive pole uses above-mentioned positive electrode, and other are with embodiment 1.
Embodiment 3
Positive electrode active materials, by nickel cobalt lithium aluminate LiNi0.82Co0.15Al0.03O2And nickle cobalt lithium manganate
LiNi0.34Co0.32Mn0.34O2Composition, is calculated in mass percent, nickel cobalt lithium aluminate 85%, nickle cobalt lithium manganate 15%.Nickel cobalt aluminic acid
The crystal grain of lithium is spherical, and D50 is 15 μm, and the crystal grain of nickle cobalt lithium manganate is that class is spherical, and D50 is 6 μm.
The preparation process of positive electrode active materials is as follows: accurately take nickel cobalt lithium aluminate and nickel cobalt mangaic acid according to mass percent
Lithium, puts into after mixing in ball grinder, and under rotating speed 80rpm, ball milling 2h, to obtain final product.
Positive electrode, by above-mentioned positive electrode active materials, white carbon black and Kynoar composition, is calculated in mass percent, positive pole
Active material 93%, white carbon black 6%, Kynoar 1%.
Lithium ion battery, positive pole uses above-mentioned positive electrode, and other are with embodiment 1.
Embodiment 4
Positive electrode active materials, by nickel cobalt lithium aluminate LiNi0.82Co0.15Al0.03O2And nickle cobalt lithium manganate
LiNi0.34Co0.32Mn0.34O2Composition, is calculated in mass percent, nickel cobalt lithium aluminate 75%, nickle cobalt lithium manganate 25%.Nickel cobalt aluminic acid
The crystal grain of lithium is spherical, and D50 is 13 μm, and the crystal grain of nickle cobalt lithium manganate is that class is spherical, and D50 is 4 μm.
The preparation process of positive electrode active materials is with embodiment 1.
Positive electrode, by above-mentioned positive electrode active materials, white carbon black and Kynoar composition, is calculated in mass percent, positive pole
Active material 95%, white carbon black 1%, Kynoar 4%.
Lithium ion battery, positive pole uses above-mentioned positive electrode, and other are with embodiment 1.
Comparative example 1
Positive electrode active materials, by nickel cobalt lithium aluminate LiNi0.8Co0.15Al0.05O2With nickle cobalt lithium manganate LiNi1/3Co1/3Mn1/ 3O2Make, be calculated in mass percent, nickel cobalt lithium aluminate 78%, nickle cobalt lithium manganate 22%；The D50 of nickel cobalt lithium aluminate is 13 μm, nickel
The D50 of cobalt manganic acid lithium is 13 μm.
The preparation of positive electrode active materials is with embodiment 1.
Positive electrode, uses above-mentioned positive electrode active materials, and other are with embodiment 1.
Lithium ion battery, positive pole uses above-mentioned positive electrode, and other are with embodiment 1.
Comparative example 2
Positive electrode active materials, by nickel cobalt lithium aluminate LiNi0.8Co0.15Al0.05O2With nickle cobalt lithium manganate LiNi1/3Co1/3Mn1/ 3O2Make, be calculated in mass percent, nickel cobalt lithium aluminate 50%, nickle cobalt lithium manganate 50%；The D50 of nickel cobalt lithium aluminate is 13 μm, nickel
The D50 of cobalt manganic acid lithium is 4 μm.
The preparation of positive electrode active materials is with comparative example 1.
Positive electrode, uses above-mentioned positive electrode active materials, and other are with comparative example 1.
Lithium ion battery, positive pole uses above-mentioned positive electrode, and other are with comparative example 1.
Test example
1, take positive electrode active materials in nickel cobalt lithium aluminate (NCA), nickle cobalt lithium manganate (NCM) and embodiment 1 and do scanning electricity
Mirror is analyzed, and scanning electron microscope (SEM) photograph is shown in that Fig. 1, Figure 1A are nickel cobalt lithium aluminate cathode material, and 1B is nickel-cobalt lithium manganate cathode material, and 1C is real
Execute positive electrode active materials in example 1.As shown in Figure 1, in embodiment 1, nickel cobalt lithium aluminate is with nickle cobalt lithium manganate mixing uniformly, nickel cobalt manganese
Acid lithium little distribution of particles between the bulky grain gap of nickel cobalt lithium aluminate, this be distributed beneficially improve pole piece compacting make
With, improve the energy density of battery further.
2, take positive electrode in nickel cobalt lithium aluminate (NCA) and embodiment 1, comparative example, do differential thermal after initial charge is complete and divide
Analysis, result is shown in Fig. 2.As shown in Figure 2, the thermal discharge of nickel cobalt lithium aluminate material self is apparently higher than embodiment 1 and comparative example, heat release
Temperature is below embodiment 1 and comparative example.And the thermal discharge of positive electrode is significantly lower than comparative example in embodiment 1, and initiates and put
Hot temperature is higher than comparative example, illustrates that in embodiment 1, the heat stability of positive electrode is more preferable compared with comparative example.
3, take positive electrode active materials in nickel cobalt lithium aluminate (NCA) and embodiment 1, comparative example and do first charge-discharge curve, with
The electric current of 0.1C carries out discharge and recharge (see Fig. 3).Result shows, the gram volume of electric discharge first of nickel cobalt lithium aluminate is 205mAh/g, real
Executing example 1 is 200mAh/g, and comparative example 1 is 191mAh/g, and comparative example 2 is only 170mAh/g.It can be seen that at nickel cobalt lithium aluminate
In be mixed into nickle cobalt lithium manganate after, the electric discharge gram volume of material is than being decreased obviously, but positive electrode active materials in embodiment 1
Electric discharge gram volume is still significantly higher than comparative example.
4, take nickel cobalt lithium aluminate (NCA) and assemble electricity in full battery, with embodiment 1 and comparative example according to method in embodiment 1
Pond together carries out room temperature loop test, test voltage 3.0～4.2V after chemical conversion constant volume, carries out discharge and recharge with 1.0C electric current and follows
Ring, the capability retention (see Fig. 4) after test loop 400 times.Result shows, the cycle performance of embodiment 1 and comparative example 2 is obvious
It is better than nickel cobalt lithium aluminate and comparative example 1.In embodiment 1, after circulating battery 400 times, capability retention is 93.2%, and cycle performance is
Excellent, and comparative example 2 is 92.3%, nickel cobalt lithium aluminate and only the 90.5% of comparative example 1.
Claims (10)
1. positive electrode active materials, it is characterised in that: by nickel cobalt lithium aluminate LiNi0.82Co0.15Al0.03O2And nickle cobalt lithium manganate
LiNi0.34Co0.32Mn0.34O2Composition, be calculated in mass percent, nickel cobalt lithium aluminate 60%～85%, nickle cobalt lithium manganate 15%～
40%.
Positive electrode active materials the most according to claim 1, it is characterised in that: the D50 of described nickel cobalt lithium aluminate is 10～15 μ
M, the D50 of nickle cobalt lithium manganate are 1～6 μm.
Positive electrode active materials the most according to claim 2, it is characterised in that: the D50 of described nickel cobalt lithium aluminate is 13 μm, nickel
The D50 of cobalt manganic acid lithium is 4 μm.
4. the preparation method of positive electrode active materials as according to any one of claims 1 to 3, it is characterised in that: according to quality hundred
Mark accurately takes nickel cobalt lithium aluminate and nickle cobalt lithium manganate, ball milling after mixing, to obtain final product.
Preparation method the most according to claim 4, it is characterised in that: the rotating speed of described ball milling is 80～120rpm, ball milling
Time 1～2h.
6. as according to any one of claims 1 to 3, positive electrode active materials at positive electrode and is prepared in lithium ion battery
Application.
Application the most according to claim 6, it is characterised in that: positive electrode is by positive electrode active materials, conductive agent and bonding
Agent forms, and is calculated in mass percent, positive electrode active materials 90%～95%, conductive agent 1%～6%, binding agent 1%～6%.
Application the most according to claim 7, it is characterised in that: described conductive agent is white carbon black or acetylene black.
9. according to the application described in claim 7 or 8, it is characterised in that: described binding agent is Kynoar.
Application the most according to claim 6, it is characterised in that: the negative active core-shell material of described lithium ion battery uses people
Making graphite or native graphite, barrier film uses polyethylene ceramic diaphragm.
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| CN106876671A (en) * | 2017-02-21 | 2017-06-20 | 张家港金盛莲能源科技有限公司 | One kind fills lithium rechargeable battery soon |
| CN108011104A (en) * | 2017-12-12 | 2018-05-08 | 桑顿新能源科技有限公司 | A kind of high compacted density lithium iron phosphate positive material and preparation method thereof |
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| CN108321384A (en) * | 2018-01-31 | 2018-07-24 | 北京国能电池科技股份有限公司 | Anode active material of lithium ion battery and positive electrode and lithium ion battery comprising it |
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| CN106876671A (en) * | 2017-02-21 | 2017-06-20 | 张家港金盛莲能源科技有限公司 | One kind fills lithium rechargeable battery soon |
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| CN108011104A (en) * | 2017-12-12 | 2018-05-08 | 桑顿新能源科技有限公司 | A kind of high compacted density lithium iron phosphate positive material and preparation method thereof |
| CN108321384A (en) * | 2018-01-31 | 2018-07-24 | 北京国能电池科技股份有限公司 | Anode active material of lithium ion battery and positive electrode and lithium ion battery comprising it |
| CN108448056A (en) * | 2018-03-15 | 2018-08-24 | 桑顿新能源科技有限公司 | A kind of preparation method of high-energy density anode pole piece and its lithium ion battery |
| CN109524642A (en) * | 2018-10-23 | 2019-03-26 | 桑顿新能源科技有限公司 | A kind of mixing tertiary cathode material and preparation method thereof |
| CN109524642B (en) * | 2018-10-23 | 2022-01-25 | 桑顿新能源科技有限公司 | Mixed ternary cathode material and preparation method thereof |
| CN110380034A (en) * | 2019-07-23 | 2019-10-25 | 合肥国轩高科动力能源有限公司 | Positive electrode material of lithium ion battery, full battery containing positive electrode material and preparation method of full battery |
| CN111370668A (en) * | 2020-03-19 | 2020-07-03 | 陆晨杰 | Pulping method of composite cathode |
| CN114709396A (en) * | 2022-04-14 | 2022-07-05 | 湖南蒙达新能源材料有限公司 | High-rate and low-temperature high-specific-energy lithium ion battery |
| CN114709396B (en) * | 2022-04-14 | 2024-02-20 | 湖南蒙达新能源材料有限公司 | Lithium ion battery with high multiplying power and low temperature and high specific energy |
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