CN108682822A - A kind of nickelic ternary material of long circulation life and preparation method thereof - Google Patents
A kind of nickelic ternary material of long circulation life and preparation method thereof Download PDFInfo
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- CN108682822A CN108682822A CN201810539641.2A CN201810539641A CN108682822A CN 108682822 A CN108682822 A CN 108682822A CN 201810539641 A CN201810539641 A CN 201810539641A CN 108682822 A CN108682822 A CN 108682822A
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- nickelic
- tertiary cathode
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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
- H01M4/366—Composites as layered products
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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
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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
- H01M4/48—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
- 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
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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
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Abstract
The invention discloses nickelic tertiary cathode materials of a kind of long circulation life and preparation method thereof, are coated to nickelic tertiary cathode material surface in such a way that wet method cladding combines mechanical fusion：Nickelic tertiary cathode material is uniformly mixed in a solvent with pre-coated object, removes solvent, mechanical fusion is carried out after calcining under oxygen, obtains the nickelic tertiary cathode material that oxide uniformly coats.The method of the present invention is simple, and material surface is evenly coated and strong adhesive force, has good protective effect to nickelic tertiary cathode material, therefore storage performance, processing performance are good, has higher specific capacity and cycle life.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical fields, and in particular to a kind of nickelic ternary of long circulation life
Material and preparation method thereof.
Background technology
There are the multiple technologies routes such as LiFePO4, ternary material and LiMn2O4 for electric powered motor anode material of lithium battery
And the phenomenon that depositing.From the point of view of these positive electrodes are with regard to energy density, cost, safety, thermal stability and cycle life, respectively there is feature
And advantage, cause dynamic lithium battery positive electrode technology path that diversification is presented.In comparison, lithium manganate battery and ferric phosphate
The theoretical energy density of lithium battery is relatively low, thus in recent years three positive electrode power batteries of higher energy density by market
Generally have an optimistic view of.The maximum tertiary cathode material of circulation is 532 types currently on the market, is secondly 111 types.Under 4.2V voltages,
111 proximate matter material gram volumes are close to 160mAh/g, and 532 proximate matter material are close to 170mAh/g.As high-energy density dynamic lithium battery is got over
More to become Developing mainstream from now on, domestic and international positive electrode manufacturing enterprise all begin one's study one after another more high-energy-density it is novel just
Pole material.
Relative to traditional tertiary cathode material (111 types and 523 types), nickelic tertiary cathode material (nickel cobalt lithium aluminate and
622,71515,811 type nickle cobalt lithium manganate) there is higher specific capacity, but since its nickel content is higher, material surface residual alkali amount
It is more, it is hygroscopic, it is easily decomposed in battery charge and discharge process, disproportionated reaction occurs, cycle performance of battery is caused to decline；While by
It is excessively high in the pH value of material, it causes the material in cell manufacturing process to be homogenized difficult, makes battery poor processability.It is asked for this
Topic, general solution are to coat nano-oxide in material surface, but traditional method for coating is extremely difficult to the equal of surface
Even cladding, and the adhesive force of coating and ontology is smaller, following process may result in falling off for coating, therefore cannot be formed
It is effectively protected.
Invention content
Higher for nickelic tertiary cathode material surface residual alkali value, processing difficulties, cycle performance be poor, easy aerogenesis etc. is asked
Topic, the present invention provide a kind of nickelic ternary material of long circulation life and preparation method thereof, are not reducing material first charge-discharge
The cyclical stability of nickel tertiary cathode material is effectively improved under conditions of capacity.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of preparation method of the nickelic ternary material of long circulation life, includes the following steps：
Step 1：Nickelic tertiary cathode material is uniformly mixed in a solvent with pre-coated object, solvent is removed, obtains pre- packet
Cover the nickelic tertiary cathode material of object package；
Step 2：The nickelic tertiary cathode material that pre-coated object wraps up is calcined under oxygen, obtains oxide cladding
Nickelic tertiary cathode material；
Step 3：The nickelic tertiary cathode material of oxide cladding is subjected to mechanical fusion, oxide is obtained and uniformly coats
Nickelic tertiary cathode material.
Further, the nickelic tertiary cathode material is nickel cobalt lithium aluminate, 622 type nickle cobalt lithium manganates, 71515 type nickel
Cobalt manganic acid lithium or 811 type nickle cobalt lithium manganates.
Further, the pre-coated object is aluminium isopropoxide, aluminum nitrate, aluminum sulfate, aluminum acetate, aluminium chloride, metatitanic acid four
It is one or more in butyl ester, isopropyl titanate and titanium tetrachloride.
Further, the solvent is one kind in ethyl alcohol, ethylene glycol, isopropanol, ethylene glycol monomethyl ether and ethylene glycol ethyl ether
Or it is a variety of.
Further, the mass ratio of pre-coated object and nickelic tertiary cathode material is (0.001- in the step 1
0.05)：1.
Further, calcination temperature is 300-750 DEG C in the step 2, calcination time 2-10h.
Further, mechanical fusion is specially mechanical agitation in the step 3, speed of agitator 2000-6000rpm, when
Between be 2-15min.
A kind of nickelic ternary material of long circulation life, is prepared using the above method.
Compared with prior art, the present invention has technique effect beneficial below：
Through pre-coated-sintering-mechanical fusion, surface coats evenly the method for the present invention, avoids lithium hydroxide, lithium carbonate
It generates, reduces the loss of active lithium-ion；Surface cladding is more secured, and coating caused by following process is avoided to fall off；After cladding
Material thermal stability it is good, insensitive to moisture, positive electrode surface quilt can be avoided under room temperature, even high temperature, high voltage
Electrolyte corrodes, and improves the cycle life of material.
Description of the drawings
Fig. 1 is the scanning electron microscopic picture for the nickel cobalt lithium aluminate that aluminum nitrate wraps up in embodiment 4；
Fig. 2 is the scanning electron microscopic picture for the nickel cobalt lithium aluminate that aluminium oxide uniformly coats in embodiment 4；
The cycle performance for the button half-cell that the nickel cobalt lithium aluminate that Fig. 3 is uniformly coated by aluminium oxide in embodiment 4 assembles
Curve.
Specific implementation mode
The present invention is described in further detail below：
A kind of preparation method of the nickelic tertiary cathode material of long circulation life, includes the following steps：
1) nickelic tertiary cathode material is uniformly mixed in a solvent with pre-coated object, removes solvent, obtains pre-coated object
The nickelic tertiary cathode material of package；The nickelic tertiary cathode material include nickel cobalt lithium aluminate, 622 type nickle cobalt lithium manganates,
71515 type nickle cobalt lithium manganates, 811 type nickle cobalt lithium manganates, the pre-coated object include aluminium isopropoxide, aluminum nitrate, aluminum sulfate, vinegar
It is one or more in sour aluminium, aluminium chloride, butyl titanate, isopropyl titanate, titanium tetrachloride；The solvent be ethyl alcohol, ethylene glycol,
One or more, and the mass ratio of pre-coated object and nickelic tertiary cathode material of isopropanol, ethylene glycol monomethyl ether, ethylene glycol ethyl ether
For (0.001-0.05)：1；The method for removing solvent includes that agitating and heating is evaporated, is spray-dried；
2) the nickelic tertiary cathode material that pre-coated object wraps up is calcined under oxygen, calcination temperature is 300-750 DEG C, is forged
The burning time is 2-10h, obtains the nickelic tertiary cathode material of oxide cladding；
3) material obtained step 2) carries out mechanical fusion, and the rotating speed of mechanical fusion is 2000-6000rpm, and the time is
2-15min obtains the nickelic tertiary cathode material that oxide uniformly coats.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
1) 622 type nickle cobalt lithium manganates and aluminium isopropoxide are uniformly mixed in ethanol with the mixture of isopropyl titanate, it is different
The mass ratio of the mixture and 622 type nickle cobalt lithium manganates of aluminium propoxide and isopropyl titanate is 0.001：1, agitating and heating is evaporated, and is obtained
622 type nickle cobalt lithium manganates of aluminium isopropoxide package；
2) 622 type nickle cobalt lithium manganates of aluminium isopropoxide package are calcined into 2h for 750 DEG C under oxygen, obtains alumina-coated
622 type nickle cobalt lithium manganates；
3) material mechanical for obtaining step 2) merges 2min, rotating speed 6000rpm, obtains aluminium oxide uniformly coats 622
Type nickle cobalt lithium manganate.
In the case where other conditions are constant, solvent can also be the mixing of ethylene glycol monomethyl ether, ethylene glycol ethyl ether or the two
Object.
Embodiment 2
1) 811 type nickle cobalt lithium manganates are uniformly mixed with aluminium isopropoxide in isopropanol, aluminium isopropoxide and 811 type nickel cobalt manganeses
The mass ratio of sour lithium is 0.05：1, agitating and heating is evaporated, and obtains 811 type nickle cobalt lithium manganates of aluminium isopropoxide package；
2) 811 type nickle cobalt lithium manganates of aluminium isopropoxide package are calcined into 10h for 300 DEG C under oxygen, obtains alumina-coated
811 type nickle cobalt lithium manganates；
3) material mechanical for obtaining step 2) merges 15min, rotating speed 2000rpm, obtains aluminium oxide uniformly coats 811
Type nickle cobalt lithium manganate.
Embodiment 3
1) 71515 type nickle cobalt lithium manganates are uniformly mixed with butyl titanate in ethylene glycol, butyl titanate and 71515
The mass ratio of type nickle cobalt lithium manganate is 0.01：1, after spray drying, obtain 71515 type nickel cobalt mangaic acids of butyl titanate package
Lithium；
2) 71515 type nickle cobalt lithium manganates of butyl titanate package are calcined into 5h for 500 DEG C under oxygen, obtains titanium oxide packet
The 71515 type nickle cobalt lithium manganates covered；
3) material mechanical for obtaining step 2) merges 10min, rotating speed 4000rpm, obtains aluminium oxide uniformly coats 811
Type nickle cobalt lithium manganate.
In the case where other conditions are constant, pre-coated object can also be aluminum sulfate, aluminum acetate, aluminium chloride, isopropyl titanate,
Titanium tetrachloride.
Embodiment 4
1) nickel cobalt lithium aluminate is uniformly mixed in ethanol with aluminum nitrate, the mass ratio of aluminum nitrate and nickel cobalt lithium aluminate is
0.002：1, after spray drying, obtain the nickel cobalt lithium aluminate of aluminum nitrate package；
2) the nickel cobalt lithium aluminate of aluminum nitrate package is calcined into 3h for 650 DEG C under oxygen, obtains the nickel cobalt aluminium of alumina-coated
Sour lithium；
3) material mechanical for obtaining step 2) merges 5min, rotating speed 5000rpm, obtains the nickel cobalt that aluminium oxide uniformly coats
Lithium aluminate.
It will be finally obtained in embodiment 4 after material is mixed with conductive agent, binder and be coated with, prepare pole piece, assembling button half
Battery carries out chemical property evaluation to material, and the results are shown in Figure 3.
Fig. 2 is the material of Fig. 1 gained after mechanical fusion, it can be seen that coating is dispersed in surface, machine before mechanical fusion
Particle adhesion phenomenon is apparent after tool fusion and has no that coating is dispersed in particle surface, illustrates the cladding of the material after mechanical fusion
Evenly, more securely.Fig. 3 can be seen that coated rear material circulation better performances, 40 circle circulation volumes are undamped.
Claims (8)
1. a kind of preparation method of the nickelic ternary material of long circulation life, which is characterized in that include the following steps：
Step 1：Nickelic tertiary cathode material is uniformly mixed in a solvent with pre-coated object, solvent is removed, obtains pre-coated object
The nickelic tertiary cathode material of package；
Step 2：The nickelic tertiary cathode material that pre-coated object wraps up is calcined under oxygen, obtains the nickelic of oxide cladding
Tertiary cathode material；
Step 3：The nickelic tertiary cathode material of oxide cladding is subjected to mechanical fusion, obtains the height that oxide uniformly coats
Nickel tertiary cathode material.
2. a kind of preparation method of the nickelic ternary material of long circulation life according to claim 1, which is characterized in that institute
The nickelic tertiary cathode material stated is nickel cobalt lithium aluminate, 622 type nickle cobalt lithium manganates, 71515 type nickle cobalt lithium manganates or 811 type nickel cobalts
LiMn2O4.
3. a kind of preparation method of the nickelic ternary material of long circulation life according to claim 1, which is characterized in that institute
The pre-coated object stated is aluminium isopropoxide, aluminum nitrate, aluminum sulfate, aluminum acetate, aluminium chloride, butyl titanate, isopropyl titanate and tetrachloro
Change one or more in titanium.
4. a kind of preparation method of the nickelic ternary material of long circulation life according to claim 1, which is characterized in that institute
It is one or more in ethyl alcohol, ethylene glycol, isopropanol, ethylene glycol monomethyl ether and ethylene glycol ethyl ether to state solvent.
5. a kind of preparation method of the nickelic ternary material of long circulation life according to claim 1, which is characterized in that institute
It is (0.001-0.05) to state the mass ratio of pre-coated object and nickelic tertiary cathode material in step 1：1.
6. a kind of preparation method of the nickelic ternary material of long circulation life according to claim 1, which is characterized in that institute
It is 300-750 DEG C to state calcination temperature in step 2, calcination time 2-10h.
7. a kind of preparation method of the nickelic ternary material of long circulation life according to claim 1, which is characterized in that institute
It is specially mechanical agitation, speed of agitator 2000-6000rpm, time 2-15min to state mechanical fusion in step 3.
8. a kind of nickelic ternary material of long circulation life, which is characterized in that using any one of claim 1-9 the method systems
It is standby to obtain.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109713252A (en) * | 2018-11-30 | 2019-05-03 | 高点(深圳)科技有限公司 | The high nickelic tertiary cathode material and its preparation method and application of electrical property consistency |
| CN110459739A (en) * | 2019-06-28 | 2019-11-15 | 河南科隆新能源股份有限公司 | A kind of positive electrode and preparation method thereof |
| CN114094093A (en) * | 2021-11-09 | 2022-02-25 | 远景动力技术(江苏)有限公司 | Cobalt-coated ternary cathode material and preparation method and application thereof |
| CN114335549A (en) * | 2022-03-10 | 2022-04-12 | 湖南长远锂科新能源有限公司 | Coating method for improving thermal stability of nickel anode material |
| EP4398340A4 (en) * | 2022-11-24 | 2024-11-06 | Tianjin B&M Science And Tech Co Ltd | Coated ternary positive electrode material, and preparation method therefor and use thereof |
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| CN114335549A (en) * | 2022-03-10 | 2022-04-12 | 湖南长远锂科新能源有限公司 | Coating method for improving thermal stability of nickel anode material |
| EP4398340A4 (en) * | 2022-11-24 | 2024-11-06 | Tianjin B&M Science And Tech Co Ltd | Coated ternary positive electrode material, and preparation method therefor and use thereof |
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