CN109244404A - A kind of preparation method of long circulating composite positive pole - Google Patents
A kind of preparation method of long circulating composite positive pole Download PDFInfo
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- CN109244404A CN109244404A CN201811063359.8A CN201811063359A CN109244404A CN 109244404 A CN109244404 A CN 109244404A CN 201811063359 A CN201811063359 A CN 201811063359A CN 109244404 A CN109244404 A CN 109244404A
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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
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- 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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- 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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
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- 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 preparation method of long circulating composite positive pole, comprising the following steps: (1) prepares AlOOH colloidal sol；(2) nanometer LiMn is prepared0.5Ni0.5O2: by micron order LiMn0.5Ni0.5O2It is mixed with pure water, sand mill grinding is added, filtering drying obtains a nanometer LiMn0.5Ni0.5O2；(3) preliminary cladding: by nanometer LiMn0.5Ni0.5O2After mixing with AlOOH colloidal sol, nickelic ternary material LiNi is added0.6Co0.2Mn0.2O2, it is uniformly mixed, then dries, obtain preliminary cladding powder；(4) it prepares composite positive pole: being crushed after being sintered and cooled in powder oxygen atmosphere that step (3) obtains.The composite material granular pattern and size distribution that the present invention prepares are controllable, and specific discharge capacity is high, and good cycling stability is at low cost.
Description
Technical field
The invention belongs to field of lithium ion battery material, more particularly to the preparation side of lithium ion cell positive ternary material
Method.
Background technique
It is the ternary layered compound of nickle cobalt lithium manganate, i.e. ternary material that anode material for lithium-ion batteries is most widely used at present
Material.High cobalt ternary material multiplying power is preferable, but safety is low and at high cost, because metallic cobalt price constantly rises violently；High manganese ternary
The cost of material is low, safety is good, but capacity is low, and high rate performance is poor；Nickelic ternary material capacity is high, but safety is low, circulation
It is poor.
Can have complementary advantages the ternary material of different proportion is compound, current main preparation method has in precursor preparation
When be settled out core-shell material or functionally gradient material (FGM), then be sintered, so that obtaining kernel is nickelic ternary, shell is low nickel ternary
Material makes it while having high capacity and high security, macrocyclic performance.But since the ternary material of different component is sintered temperature
Degree is different, has the several hundred degree of phase difference, causes the performance of this core-shell material that cannot always reach expected.Another relatively common side
Method is to grind low nickel ternary material and nickelic ternary material in grinder, compound to the two, but process of lapping can be to material
It is broken that material causes physics, and the compound uniformity and degree are uncontrollable, and expection is not achieved in the composite property that the method is prepared.
It is widely used nickelic ternary material the requirement of cell high-capacity at present, but its cycle performance is poor.
Summary of the invention
In view of the drawbacks of the prior art, the present invention provides a kind of preparation method of long circulating composite positive pole, obtains
Anode material discharging specific capacity height, good cycling stability.
A kind of preparation method of long circulating composite positive pole, comprising the following steps:
(1) AlOOH colloidal sol is prepared；
(2) nanometer LiMn is prepared0.5Ni0.5O2: by micron order LiMn0.5Ni0.5O2It mixes, adds by solid content 20%-50% with pure water
Enter sand mill grinding, filtering drying obtains a nanometer LiMn0.5Ni0.5O2；
(3) preliminary cladding: the nanometer LiMn that step (2) is obtained0.5Ni0.5O2The AlOOH colloidal sol mixing obtained with step (1) is equal
After even, nickelic ternary material LiNi is added0.6Co0.2Mn0.2O2, it is uniformly mixed, then dries, obtain preliminary cladding powder；
(4) prepare composite positive pole: in the powder oxygen atmosphere that step (3) is obtained 850-910 DEG C sintering 2-6 hours,
It crushed 400 mesh after cooling.
Preferably, preparation AlOOH colloidal sol is specific as follows in step (1): aluminium isopropoxide being dissolved in pure water and forms mass concentration
For the aqueous solution of the aluminium isopropoxide of 5-10%, 3 ~ 5h is continuously stirred under 80-90 DEG C of water bath condition, concentration is then added dropwise thereto
For the HNO of 0.5-1mol/L3Solution, control pH value to 2-5, continuing stirring makes its aging 15-20h, obtains AlOOH colloidal sol.
Preferably, nanometer LiMn in step (3)0.5Ni0.5O2, the quality in AlOOH colloidal sol containing Al, nickelic ternary material
LiNi0.6Co0.2Mn0.2O2Mass ratio be (0.5-3): (0.05-0.5): 100.
Preferably, the time ground in step (2) is 15-60min.
Preferably, micron order LiMn described in step (2)0.5Ni0.5O2Partial size at 1-100 μm.
Preferably, nanometer LiMn in step (3)0.5Ni0.5O2, the quality in AlOOH colloidal sol containing Al, nickelic ternary material
LiNi0.6Co0.2Mn0.2O2Mass ratio be (0.5-3): 0.2:100.
Preferably, the temperature being sintered in step (4) is 880 DEG C.
The LiMn used in the present invention0.5Ni0.5O2And LiNi0.6Co0.2Mn0.2O2For the material sold in existing market.
Advantages of the present invention:
Method provided by the invention, by Aluminum sol by nanometer LiMn0.5Ni0.5O2Uniformly it is adhered in LiNi0.6Co0.2Mn0.2O2Table
Face, and handled by short time high temperature, keep two materials completely compound.And the Aluminum sol as adhesive, after high-temperature process
As Al2O3, the reaction of electrolyte and material can be prevented to extend material circulation performance in inside battery.Present invention preparation
Composite material granular pattern and size distribution out is controllable, and specific discharge capacity is high, and good cycling stability is at low cost.
Detailed description of the invention
Fig. 1 is nanometer LiMn prepared by the embodiment of the present invention 10.5Ni0.5O2Scanning electron microscope (SEM) photograph.
Fig. 2 is the scanning electron microscope (SEM) photograph of long circulating composite positive pole prepared by the embodiment of the present invention 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of long circulating composite positive pole prepared by the embodiment of the present invention 2.
Fig. 4 is the scanning electron microscope (SEM) photograph of long circulating composite positive pole prepared by the embodiment of the present invention 3.
Fig. 5 is the charging and discharging curve figure of the long circulating composite positive pole of 1-3 of embodiment of the present invention preparation.
Fig. 6 is the cyclic curve figure of the long circulating composite positive pole of 1-3 of embodiment of the present invention preparation.
Specific embodiment
Embodiment 1
1. a kind of preparation method of long circulating composite positive pole, comprising the following steps:
(1) it prepares AlOOH colloidal sol: 20.4g aluminium isopropoxide is dissolved in the water-soluble of the aluminium isopropoxide that pure water formation mass concentration is 5%
Liquid continuously stirs 4h under 85 DEG C of water bath conditions, and the HNO that concentration is 0.5mol/L is then added dropwise thereto3Solution controls pH value
To 3, continuing stirring makes its aging 20h, obtains AlOOH colloidal sol；
(2) nanometer LiMn is prepared0.5Ni0.5O2: the LiMn by partial size at 1-100 μm0.5Ni0.5O2It is mixed by solid content 30% with pure water
It closes, sand mill is added and grinds 30min, filtering drying obtains a nanometer LiMn0.5Ni0.5O2；
(3) preliminary cladding: the nanometer LiMn that step (2) is obtained0.5Ni0.5O2The AlOOH colloidal sol mixing obtained with step (1) is equal
After even, nickelic ternary material LiNi is added0.6Co0.2Mn0.2O2, it is uniformly mixed, then dries, obtain preliminary cladding powder；Its
In, nanometer LiMn0.5Ni0.5O2, the quality in AlOOH colloidal sol containing Al, nickelic ternary material LiNi0.6Co0.2Mn0.2O2Mass ratio
For 1:0.2:100；
(4) it prepares composite positive pole: being sintered 4 hours in the powder oxygen atmosphere that step (3) is obtained at 880 DEG C, after cooling
It crushed 400 mesh.
Embodiment 2
1. a kind of preparation method of long circulating composite positive pole, comprising the following steps:
(1) it prepares AlOOH colloidal sol: 20.4g aluminium isopropoxide is dissolved in the water-soluble of the aluminium isopropoxide that pure water formation mass concentration is 10%
Liquid continuously stirs 5h under 80 DEG C of water bath conditions, and the HNO that concentration is 1mol/L is then added dropwise thereto3Solution, control pH value is extremely
5, continuing stirring makes its aging 15h, obtains AlOOH colloidal sol；
(2) nanometer LiMn is prepared0.5Ni0.5O2: the LiMn by partial size at 1-100 μm0.5Ni0.5O2It is mixed by solid content 20% with pure water
It closes, sand mill is added and grinds 15min, filtering drying obtains a nanometer LiMn0.5Ni0.5O2；
(3) preliminary cladding: the nanometer LiMn that step (2) is obtained0.5Ni0.5O2The AlOOH colloidal sol mixing obtained with step (1) is equal
After even, nickelic ternary material LiNi is added0.6Co0.2Mn0.2O2, it is uniformly mixed, then dries, obtain preliminary cladding powder；Its
In, nanometer LiMn0.5Ni0.5O2, the quality in AlOOH colloidal sol containing Al, nickelic ternary material LiNi0.6Co0.2Mn0.2O2Mass ratio
For 0.5:0.05:100；
(4) it prepares composite positive pole: being sintered 2 hours in the powder oxygen atmosphere that step (3) is obtained at 850 DEG C, after cooling
It crushed 400 mesh.
Embodiment 3
1. a kind of preparation method of long circulating composite positive pole, comprising the following steps:
(1) it prepares AlOOH colloidal sol: aluminium isopropoxide is dissolved in the aqueous solution that pure water forms the aluminium isopropoxide that mass concentration is 10%,
3h is continuously stirred under 90 DEG C of water bath conditions, the HNO that concentration is 1mol/L is then added dropwise thereto3Solution, control pH value to 2, after
Continuous stirring makes its aging 20h, obtains AlOOH colloidal sol；
(2) nanometer LiMn is prepared0.5Ni0.5O2: the LiMn by partial size at 1-100 μm0.5Ni0.5O2It is mixed by solid content 50% with pure water
It closes, sand mill is added and grinds 60min, filtering drying obtains a nanometer LiMn0.5Ni0.5O2；
(3) preliminary cladding: the nanometer LiMn that step (2) is obtained0.5Ni0.5O2The AlOOH colloidal sol mixing obtained with step (1) is equal
After even, nickelic ternary material LiNi is added0.6Co0.2Mn0.2O2, it is uniformly mixed, then dries, obtain preliminary cladding powder；Its
In, nanometer LiMn0.5Ni0.5O2, the quality in AlOOH colloidal sol containing Al, nickelic ternary material LiNi0.6Co0.2Mn0.2O2Mass ratio
For 3:0.5:100；
(4) it prepares composite positive pole: being sintered 6 hours in the powder oxygen atmosphere that step (3) is obtained at 910 DEG C, after cooling
It crushed 400 mesh.
One, performance detection
1. nanometer LiMn prepared by step (2) in embodiment 10.5Ni0.5O2Scanning electron microscope is done, sees Fig. 1 by embodiment 1-3 system
Standby positive electrode does scanning electron microscope, sees Fig. 2-4 respectively；As seen from the figure, nanometer LiMn0.5Ni0.5O2Particle uniformly, cladding after
Material is evenly coated；
2. charging and discharging curve and the cyclic curve difference of embodiment 1-3 resulting materials are as shown in Figure 5 and Figure 6, it is known that, embodiment 1
The discharge capacity of preparation-obtained positive electrode is 175.6mAh/g, and first run efficiency for charge-discharge is 89%, capacity after 50 circulations
Conservation rate is 96%；The discharge capacity of the preparation-obtained positive electrode of embodiment 2 is 175.1mAh/g, first run efficiency for charge-discharge
It is 88.7%, capacity retention ratio is 97% after 50 circulations；The discharge capacity of the preparation-obtained positive electrode of embodiment 3 is
174mAh/g, first run efficiency for charge-discharge are 88%, and capacity retention ratio is 99% after 50 circulations.
Claims (7)
1. a kind of preparation method of long circulating composite positive pole, it is characterised in that: the following steps are included:
(1) AlOOH colloidal sol is prepared；
(2) nanometer LiMn is prepared0.5Ni0.5O2: by micron order LiMn0.5Ni0.5O2It mixes, is added by solid content 20%-50% with pure water
Sand mill grinding, filtering drying obtain a nanometer LiMn0.5Ni0.5O2；
(3) preliminary cladding: the nanometer LiMn that step (2) is obtained0.5Ni0.5O2The AlOOH colloidal sol mixing obtained with step (1) is equal
After even, nickelic ternary material LiNi is added0.6Co0.2Mn0.2O2, it is uniformly mixed, then dries, obtain preliminary cladding powder；
(4) prepare composite positive pole: in the powder oxygen atmosphere that step (3) is obtained 850-910 DEG C sintering 2-6 hours,
It crushed 400 mesh after cooling.
2. the preparation method of long circulating composite positive pole according to claim 1, it is characterised in that: preparation in step (1)
AlOOH colloidal sol is specific as follows: aluminium isopropoxide is dissolved in the aqueous solution that pure water forms the aluminium isopropoxide that mass concentration is 5-10%,
3 ~ 5h is continuously stirred under 80-90 DEG C of water bath condition, and the HNO that concentration is 0.5-1mol/L is then added dropwise thereto3Solution controls pH
For value to 2-5, continuing stirring makes its aging 15-20h, obtains AlOOH colloidal sol.
3. the preparation method of long circulating composite positive pole according to claim 1, it is characterised in that: nanometer in step (3)
LiMn0.5Ni0.5O2, the quality in AlOOH colloidal sol containing Al, nickelic ternary material LiNi0.6Co0.2Mn0.2O2Mass ratio be (0.5-
3): (0.05-0.5): 100.
4. the preparation method of long circulating composite positive pole according to claim 1, it is characterised in that: grinding in step (2)
Time be 15-60min.
5. the preparation method of long circulating composite positive pole according to claim 1, it is characterised in that: described in step (2)
Micron order LiMn0.5Ni0.5O2Partial size at 1-100 μm.
6. the preparation method of long circulating composite positive pole according to claim 3, it is characterised in that: nanometer in step (3)
LiMn0.5Ni0.5O2, the quality in AlOOH colloidal sol containing Al, nickelic ternary material LiNi0.6Co0.2Mn0.2O2Mass ratio be (0.5-
3): 0.2:100.
7. the preparation method of long circulating composite positive pole according to claim 1, it is characterised in that: sintering in step (4)
Temperature be 880 DEG C.
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