CN109742377A - A kind of method that nickelic tertiary cathode material surface is modified - Google Patents

A kind of method that nickelic tertiary cathode material surface is modified Download PDF

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Publication number
CN109742377A
CN109742377A CN201910043577.3A CN201910043577A CN109742377A CN 109742377 A CN109742377 A CN 109742377A CN 201910043577 A CN201910043577 A CN 201910043577A CN 109742377 A CN109742377 A CN 109742377A
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cathode material
tertiary cathode
nickelic
nickelic tertiary
modified
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CN201910043577.3A
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CN109742377B (en
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夏阳
陈安琪
王坤
张文魁
吴海军
黄辉
毛秦钟
吉同棕
甘永平
张俊
梁初
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Zhejiang Haichuang Lithium Battery Technology Co ltd
Zhejiang University of Technology ZJUT
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Zhejiang Meidu Haichuang Lithium Electricity Technology Co ltd
Zhejiang University of Technology ZJUT
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Publication of CN109742377A publication Critical patent/CN109742377A/en
Priority to PCT/CN2020/071713 priority patent/WO2020147671A1/en
Priority to JP2021540849A priority patent/JP7236631B2/en
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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
    • 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
    • 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
    • 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
    • H01M4/48—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
    • 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
    • H01M4/48—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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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 present invention provides a kind of nickelic tertiary cathode material surface modifying methods, nickelic tertiary cathode material is put into plasma generator, arc gas has been used as using carbon dioxide gas, tertiary cathode material is surface-treated in carbon dioxide plasma atmosphere, one layer of lithium carbonate and carbon coating layer can be constructed in its surface in situ, active material can be not only effectively isolated directly to contact with electrolyte, enhance the electronic conductivity of its surface and interface, chemical stability exposed for a long time in humid air can be greatly improved simultaneously, help to improve the structural stability and post-production of material.Tertiary cathode material rough surface (tree root shape) after this method is surface-treated, processing performance, cyclical stability, capacity retention ratio and high rate performance are all obviously improved.The surface treatment method has simple process, easy to operate, rapidly and efficiently, low in cost, the characteristics of remarkable in economical benefits.

Description

A kind of method that nickelic tertiary cathode material surface is modified
Technical field
The present invention relates to a kind of methods that nickelic tertiary cathode material surface is modified, belong to anode material for lithium-ion batteries skill Art field.
Background technique
Extensive use has been obtained in lithium ion battery in portable electronic device, household electrical appliance and electric tool. However, the application in electric car field also fails to reach this achievement, it is primarily due to the high cost of lithium ion battery and increases The cost of electric car is added, the use demand of user is not achieved in specific energy density, limits the development of electric car.Currently, Lithium ion battery cost and energy density depend greatly on the performance of positive electrode, this is most heavy and most expensive group Part.Nickelic tertiary cathode material has many advantages, such as specific discharge capacity height and cheap, it is considered to be next-generation lithium ion battery Positive electrode and have received widespread attention.However, nickelic positive electrode is very sensitive to the water in air, easily and in air Moisture reaction, in Surface Creation lithium hydroxide, to cause material surface rotten, cause subsequent anode sizing agent preparation it is difficult, The problems such as positive electrode capacity decaying and cyclical stability variation.Therefore, not surface treated nickelic positive electrode is to storage Condition and post-production environment have more harsh requirement, the storage cost of material are not only increased, after also increasing material Continuous difficulty of processing.To solve the above-mentioned problems, researcher would generally using indifferent oxide method for coating to nickelic ternary just The surface of pole material is modified and modifies, so as to improve structural stability and cyclical stability.
Chinese patent CN106207128A discloses a kind of Zr (OH)4Coat the preparation side of nickel cobalt aluminium tertiary cathode material Method, comprising the following steps: (1) prepare the alcoholic solution of soluble zirconium alkoxide；(2) alcohol-water solution is prepared, and it is rapid that progress is slowly added dropwise (1) in solution made from；(3) ultrasound, washing, suction filtration, drying, obtain amorphous Zr (OH)4Powder；(4) by ternary material and Zr(OH)4Powder obtains Zr (OH) by ball milling mixing4Tertiary cathode material after coating modification.
Chinese patent CN103178258A discloses a kind of preparation of modified nickel-cobalt-manganternary ternary anode material of alumina-coated Method comprising: (1) it prepares presoma: water-soluble metal nickel salt, cobalt salt and manganese salt is made into mixed solution, with precipitating reagent, shape Looks controlling agent is added drop-wise in reaction vessel together and the pH value and reaction temperature of control system, is filtered, washed after reaction and very Sky is dry, obtains presoma；(2) it prepares the presoma of alumina-coated: presoma, water-soluble aluminum salt and equal powder is dispersed in In deionized water, warming while stirring to equal powder is hydrolyzed, and Al (OH) is obtained by filtration3The presoma of cladding, is placed in sintering furnace Roasting obtains Al2O3The precursor powder of cladding；(3) by Al2O3The precursor powder of cladding is uniformly mixed with lithium salts powder, high Temperature calcining obtains the modified nickel-cobalt-manganternary ternary anode material of alumina-coated of layered crystal structure.
As previously mentioned, mainly having solid phase and liquid phase coating sintering two at present to nickelic positive electrode surface coating modification method Kind.Solid phase cladding sintering process clad uniformity obtained is poor, and the binding force between clad and matrix is weaker, is recycling In the process since the anisotropy volume expansion of positive electrode causes clad to rupture, continues to lead to material degradation, influence Material circulation performance.Liquid phase method mostly uses greatly water as solvent, however water can react with nickelic tertiary cathode material, cause Lithium is lost, and eventually leads to material capacity decline.Lead to capacitance loss with liquid phase coating for being evenly coated property of solid phase surface is poor The problems such as, the present invention provides a kind of plasma surface modification processing method, passes through on nickelic tertiary cathode material surface gas-solid Reactive mode constructs one layer of lithium carbonate and carbon coating layer in situ, can not only be effectively isolated active material and directly connect with electrolyte Touching, enhances the electronic conductivity of its surface and interface, while can greatly improve and be exposed in humid air the chemistry after long-time surely It is qualitative, help to improve the structural stability and post-production of material.This method has simple relative to traditional method for coating It is convenient, rapidly and efficiently, the advantages such as low in cost.
Summary of the invention
The present invention is insufficient in the prior art in order to solve, and provides a kind of side that nickelic tertiary cathode material surface is modified Method.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of method that nickelic tertiary cathode material surface is modified, described method includes following steps:
S1, nickelic tertiary cathode material is laid in container, is put into plasma generator cavity, open vacuum pump, Plasma generator cavity is evacuated to vacuum；
S2, the dry arc gas that rises is passed through in cavity, so that cavity air pressure is maintained 500~700Pa, keeps 20~60s, Arc gas extraction will be played again, and chamber vacuum degree is made to be maintained at 40~50Pa；
S3, plasma generator is opened, regulation power after reaction 0.5~120 minute, can be obtained what surface was modified Nickelic tertiary cathode material.
Preferably, the chemical formula of nickelic tertiary cathode material described in step S1 is LiNi(1-x-y)CoxMyO2, wherein x + y≤0.7, M are Mn or Al.
Preferably, the chemical formula of the nickelic tertiary cathode material is LiNi0.9Co0.05Mn0.05O2、 LiNi0.8Co0.1Mn0.1O2、LiNi0.6Co0.2Mn0.2O2、LiNi0.85Co0.1Al0.05O2Or LiNi0.5Co0.2Mn0.3O2。
Preferably, described arc gas is carbon dioxide.
Preferably, the tiling of nickelic tertiary cathode material is in step S1 with a thickness of 0.3mm~10mm.
Preferably, the power of step S3 plasma generator is 5~2000W.
Present invention also provides a kind of lithium ion battery, the positive electrode of the lithium ion battery is side described herein The modified nickelic tertiary cathode material in surface made from method.
The beneficial effects of the present invention are:
Using plasma surface treatment can answering in one layer of lithium carbonate of nickelic tertiary cathode material surface construction and carbon Clad is closed, lithium carbonate is electrochemically inactive material, and nickelic tertiary cathode material can be made to be isolated with the steam in air, avoid it It is reacted with steam and generates lithium hydroxide, destroy its surface and interface structure, so as to improve its adding in subsequent electrode piece production process Work；At the same time, the surface and interface electronic conductivity of nickelic tertiary cathode material can be improved in a small amount of carbon present in clad, Be conducive to improve the circulation and high rate performance of battery；This method simple process, processing is convenient, rapidly and efficiently, remarkable in economical benefits.
Detailed description of the invention
Fig. 1 is the SEM spectrum for the modification tertiary cathode material that embodiment 1 obtains；
Fig. 2 is the XRD spectrum for the modification tertiary cathode material that embodiment 1 obtains；
Fig. 3 be the battery for preparing of embodiment 1 under 20mA/g current density before charging and discharging curve three times；
Fig. 4 is that battery prepared by embodiment 1 first activates three circulations under 20mA/g current density, then in 100mA/g 200 charge and discharge cycles curves are recycled under current density.
Specific embodiment
Below by embodiment, in conjunction with attached drawing, explanation is further described to technical solution of the present invention.
Embodiment 1:
Preparation includes the battery of nickelic tertiary cathode material:
Step 1: the nickelic tertiary cathode material that preparation surface is modified
A kind of method that nickelic tertiary cathode material surface is modified, described method includes following steps:
S1, by 2g tertiary cathode LiNi0.83Co0.085Mn0.085O2Material is laid in quartz boat, and control tiling thickness exists 0.5mm is put into plasma generator, and reactor cavity is evacuated to vacuum；
S2, dry carbon dioxide gas is passed through in reactor cavity, cavity air pressure is made to maintain 550Pa, kept 20s, then carbon dioxide gas is extracted out, so that chamber vacuum degree is maintained at 40Pa；
S3, plasma generator, regulation power 18W are opened, reaction after ten minutes, can be obtained the modified height in surface Nickel tertiary cathode material.
Step 2: the preparation of battery
It S4, is in mass ratio that 90:5:5 weighs the nickelic tertiary cathode material that the surface of acquisition is modified, conductive agent (acetylene It is black) and binder (Kynoar), it is uniformly mixed, adds suitable -2 pyrrolidones of 1- methyl (NMP) and make solvent, it is mechanical 3h is stirred, the slurry with certain viscosity is obtained；
S5, the resulting slurry of step S4 is coated uniformly on clean smooth aluminium foil, coating thickness is 200 μm, 120 Dry 12h in DEG C vacuum drying oven, the pole piece that drying backlash is 15mm at diameter, with 18MPa pressure compaction, as anode pole piece, It is spare；
S6, anode cover, anode pole piece, diaphragm, electrolyte, lithium piece, nickel foam, electrolyte, negative electrode casing are pressed in glove box Sequence be assembled into CR2025 type button cell, wherein the model Celgard 2300 of diaphragm, electrolyte are 1mol L- 1LiPF6/ EC+DEC (volume ratio 1:1).
Step 3: the test of chemical property
Chemical property is tested after battery made from second step is shelved 12h:
Certain current density is used to carry out charge-discharge test (3 times with current density for the electric current of 20mA/g to battery Active cell then carries out charge and discharge cycles with the electric current that current density is 100mA/g), voltage range is 3~4.2V, charge and discharge The time interval of electricity is 5min.The performance of lithium ion battery of material prepared is as follows；
Attached drawing 1 is the LiNi in the present embodiment0.83Co0.085Mn0.085O2Tertiary cathode material treated SEM spectrum, figure Material surface becomes coarse after spectrum is shown in carbon dioxide corona treatment, but spherical morphology has not been changed；
Attached drawing 2 is the LiNi in the present embodiment0.83Co0.085Mn0.085O2Tertiary cathode material treated XRD spectrum, figure No change has taken place for material layer structure after spectrum is shown in carbon dioxide corona treatment；
Attached drawing 3 be the present embodiment in battery under the current density of 20mA/g, voltage range be 3~4.2V it is preceding three times Charging and discharging curve, discharge capacity is 194mA h/g for the first time；
Attached drawing 4 is that the battery in the present embodiment first activates 3 times under the current density of 20mA/g, then 100mA/g's Cycle performance figure under current density, after 200 circulations, discharge capacity still has 158mA h/g, capacity retention ratio 86.8% (opposite the 4th charge and discharge).
Embodiment 2-5
According to the experimental procedure of embodiment 1, change the time of surface treatment, the surface treatment time difference of embodiment 2~5 For 5min, 20min, 30min, the step of 60min (0min is control group, i.e., is not surface-treated), assembled battery same embodiment 1, the chemical property of surveyed battery is as shown in table 1:
Table 1: influence of the carbon dioxide plasma treatment time to material circulation performance
Although the tertiary cathode material as can be seen from Table 1 after plasma surface treatment is in discharge capacity for the first time Slightly decay, but the properties of sample on capacity retention ratio than not being surface-treated is more excellent (but should not handle the long time), says Bright plasma surface modification processing can be improved the cyclical stability of material, which is subsequent tertiary cathode material Surface modification treatment provides new thinking.
Embodiment 6-7
According to the experimental procedure of embodiment 1, change the power of plasma generator, the plasma hair of embodiment 6 and 7 The power of raw device is respectively 6.8W and 10.5W, in the case where other conditions are constant, with embodiment 1, institute the step of assembled battery The chemical property for surveying battery is as shown in table 2:
Table 2: influence of the carbon dioxide corona treatment power to material circulation performance
The nickelic tertiary cathode material after plasma surface treatment compares plasma surface treatment as can be seen from Table 2 It is preceding all to increase on capacity retention ratio and cyclical stability, illustrate that plasma surface modification processing can be improved material Cyclical stability.
Embodiment described above is preferred version of the invention, is not intended to limit the present invention in any form, There are also other variants and remodeling on the premise of not exceeding the technical scheme recorded in the claims.

Claims (7)

1. a kind of method that nickelic tertiary cathode material surface is modified, which is characterized in that described method includes following steps:
S1, nickelic tertiary cathode material is laid in container, is put into plasma generator cavity, open vacuum pump, it will Plasma generator cavity is evacuated to vacuum；
S2, the dry arc gas that rises is passed through in cavity, cavity air pressure is made to maintain 500~700Pa, keep 20~60s, then will Arc gas extraction is played, chamber vacuum degree is made to be maintained at 40~50Pa；
S3, plasma generator is opened, regulation power after reaction 0.5~120 minute, can be obtained the nickelic of surface modification Tertiary cathode material.
2. the modified method in nickelic tertiary cathode material surface according to claim 1, which is characterized in that institute in step S1 The chemical formula for stating nickelic tertiary cathode material is LiNi(1-x-y)CoxMyO2, x+y≤0.7, M are Mn or Al.
3. the modified method in nickelic tertiary cathode material surface according to claim 2, which is characterized in that described nickelic three The chemical formula of first positive electrode is LiNi0.9Co0.05Mn0.05O2、LiNi0.8Co0.1Mn0.1O2、LiNi0.6Co0.2Mn0.2O2、 LiNi0.85Co0.1Al0.05O2Or LiNi0.5Co0.2Mn0.3O2。
4. the modified method in nickelic tertiary cathode material surface according to claim 1, which is characterized in that the starting the arc gas Body is carbon dioxide.
5. the modified method in nickelic tertiary cathode material surface according to claim 1, which is characterized in that high in step S1 The tiling of nickel tertiary cathode material is with a thickness of 0.3mm~10mm.
6. the modified method in nickelic tertiary cathode material surface according to claim 1, which is characterized in that step S3 is medium The power of plasma generator is 5~2000W.
7. a kind of lithium ion battery, which is characterized in that the lithium ion battery includes the side of 1~6 any one of right The modified nickelic tertiary cathode material in the surface of method preparation.
CN201910043577.3A 2019-01-17 2019-01-17 Method for surface modification of high-nickel ternary positive electrode material Active CN109742377B (en)

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PCT/CN2020/071713 WO2020147671A1 (en) 2019-01-17 2020-01-13 Method for modifying surface of high nickel ternary positive electrode material
JP2021540849A JP7236631B2 (en) 2019-01-17 2020-01-13 Nickel ternary positive electrode material surface modification method

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CN110330059A (en) * 2019-06-25 2019-10-15 浙江工业大学 A kind of sintering process of the nickelic positive electrode of high stability lithium ion
CN110350165A (en) * 2019-06-25 2019-10-18 浙江工业大学 A kind for the treatment of process promoting nickelic positive electrode stability and electric conductivity
CN110350167A (en) * 2019-06-25 2019-10-18 浙江工业大学 A kind of preparation process improving nickelic positive electrode cycle performance and electric conductivity
CN110350166A (en) * 2019-06-25 2019-10-18 浙江工业大学 A method of improving tertiary cathode material stability and processability
CN110233252A (en) * 2019-06-25 2019-09-13 浙江工业大学 A kind of sodium-ion battery positive material surface modifying method
WO2020259436A1 (en) * 2019-06-25 2020-12-30 浙江工业大学 Method for improving stability and processability of ternary positive electrode material
CN110714195A (en) * 2019-08-26 2020-01-21 浙江工业大学 Surface modification method for metal lithium
CN111628151A (en) * 2020-06-09 2020-09-04 湖南长远锂科股份有限公司 Surface modification method of ternary cathode material
CN111883748A (en) * 2020-06-29 2020-11-03 华南理工大学 Method for coating oxide film on surface of lithium ion battery anode powder material
CN112467066A (en) * 2020-11-25 2021-03-09 四川虹微技术有限公司 Pulping method of high-nickel ternary material
CN113044893A (en) * 2021-03-12 2021-06-29 电子科技大学 Method for carrying out carbon coating modification on high-nickel ternary material
CN113764633A (en) * 2021-07-21 2021-12-07 广西师范大学 Surface modified lithium ion battery positive electrode material and preparation method thereof
CN114229921A (en) * 2021-12-22 2022-03-25 西南科技大学 Al2O3-ZrO2Coated lithium-rich manganese-based positive electrode material and preparation method thereof
CN114229921B (en) * 2021-12-22 2023-09-15 西南科技大学 Al 2 O 3 -ZrO 2 Coated lithium-rich manganese-based positive electrode material and preparation method thereof
CN114613988A (en) * 2022-04-01 2022-06-10 湖南桑瑞新材料有限公司 Preparation method of high-stability ternary cathode material, ternary cathode material and lithium ion battery
CN114613988B (en) * 2022-04-01 2022-09-20 湖南桑瑞新材料有限公司 Preparation method of high-stability ternary cathode material, ternary cathode material and lithium ion battery
CN114988492A (en) * 2022-05-31 2022-09-02 西安合升汇力新材料有限公司 Nickel-rich ternary cathode material and preparation method and application thereof

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