CN109980188A - A kind of nickel-cobalt lithium manganate cathode material and preparation method thereof coating aluminum phosphate - Google Patents
A kind of nickel-cobalt lithium manganate cathode material and preparation method thereof coating aluminum phosphate Download PDFInfo
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- CN109980188A CN109980188A CN201711446933.3A CN201711446933A CN109980188A CN 109980188 A CN109980188 A CN 109980188A CN 201711446933 A CN201711446933 A CN 201711446933A CN 109980188 A CN109980188 A CN 109980188A
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- lithium manganate
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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
- H01M4/362—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
- 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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
Abstract
The invention discloses a kind of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate, chemical expressions are as follows: LiaNixCoyMnzPcO2, wherein 1≤a≤1.2,0.3≤x≤0.98,0.01≤y≤0.6,0.001≤z≤0.2,0.0001≤c≤0.01；The invention also discloses a kind of preparation methods of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate；The present invention by with aluminum soluble salt be the source Al, using soluble phosphate as precipitating reagent, by control crystal chemistry plating method in positive electrode surface one layer of AlPO of uniform plating4Clad, this method is simple to operation, accurately controls AlPO4Covering amount, and during cladding by surfactant solve sedimentation problem, keep clad uniform and thin, improve the cycle life and security performance of positive electrode.
Description
Technical field
The invention belongs to battery material technical fields, and in particular to a kind of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate
And preparation method thereof.
Background technique
Nickel-cobalt-manganese ternary anode material for lithium-ion batteries is due to energy density with higher and relatively simple system
Standby technique is widely used in IT product and new-energy automobile field, but nickle cobalt lithium manganate (LNCA) is due to structural stability
Not good enough, high price nickel is easy to react with electrolyte, the decomposition of electrolyte is caused, and release gas, to the cycle life and peace of material
Full property causes great harm；Generally improved regarding to the issue above using surface coated mode, positive electrode surface cladding
Chemically inert substance positive electrode and electrolyte are effectively isolated, avoid reacting for high price nickel ion and electrolyte, protect
The stability for holding anode with electrolyte, to improve the cycle life and security performance of material.
AlPO4Cladding there is obvious action, but simultaneously because packet to the stability for improving positive electrode and electrolyte
What is covered is typically all the substance of non-electroactive, and the specific discharge capacity for mutually coping with material affects, if cladding
To measure excessively high, discharge capacity will significantly reduce, if covering amount is insufficient, the stability of material cannot effectively improve, because
This, it is to realize that specific discharge capacity and stability reach balance that covering material can be uniform and thin, which is coated on positive electrode surface,
Key factor, and AlPO is prevented during cladding4Precipitating.
Summary of the invention
The object of the present invention is to provide a kind of nickel-cobalt lithium manganate cathode materials for coating aluminum phosphate, by positive electrode
Surface coats aluminum phosphate, in the stability for solving to ensure that positive electrode while specific discharge capacity is too low.
It is a further object to provide a kind of preparation methods of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate.
The technical scheme adopted by the invention is that:
A kind of nickel-cobalt lithium manganate cathode material coating aluminum phosphate, chemical expression are as follows: LiaNixCoyMnzPcO2,
In, 1≤a≤1.2,0.3≤x≤0.98,0.01≤y≤0.6,0.001≤z≤0.2,0.0001≤c≤0.01.
The features of the present invention also characterized in that
The doped metallic elements in positive electrode, chemical expression are as follows: LiaNixCoyMnzPcRbO2, wherein b=4/
3-a/3-x-y-z, 0.00001≤b≤0.03, R are metallic element, and the metallic element is the element other than nickel, cobalt, manganese
One or more combinations of metallic element in periodic table.
A kind of preparation method for the nickel-cobalt lithium manganate cathode material coating aluminum phosphate, is specifically implemented according to the following steps:
Step 1, nickel-cobalt lithium manganate cathode material is weighed respectively, measures aluminum salt solution and phosphate solution；
Step 2, the weighed nickel-cobalt lithium manganate cathode material of the step 1 is dispersed in water, and is heated, obtain nickel cobalt
Lithium manganate cathode slurry；
Step 3, aluminum salt solution and phosphate solution that the step 1 measures are added to according to certain speed cocurrent
It in the nickle cobalt lithium manganate slurry of step 2 and stirs, while surfactant is added；
Step 4, after the completion of charging by the nickle cobalt lithium manganate slurries filtration of the step 3, drying, be heat-treated up to cladding phosphorus
The nickel-cobalt lithium manganate cathode material of sour aluminium.
The features of the present invention also characterized in that
Nickel in nickel-cobalt lithium manganate cathode material in the step 1, cobalt, manganese the ratio between mole be (0.3-0.98): (0.01-
0.6):(0.001-0.1)。
The mass ratio of nickel-cobalt lithium manganate cathode material and phosphate solution is 100:(0.01-1 in the step 1), aluminium salt
The molar ratio of solution and phosphate solution is 1:(1.1-1.2).
The concentration of aluminum salt solution is 0.05mol/L-0.5mol/L in the step 1, and the concentration of the phosphate solution is
0.1mol/L-1mol/L。
The mass ratio of nickel-cobalt lithium manganate cathode material and water is 1:(3-10 in the step 2), the temperature of heating is 30-90
℃。
Mixing speed is 50-200r/min in the step 3.
The additive amount of surfactant is the 1%-5% of nickle cobalt lithium manganate anode sizing agent quality in the step 3.
In the step 4 300-700 DEG C at a temperature of be heat-treated 1-10h.
Compared with prior art, the present invention with aluminum soluble salt by, for the source Al, using soluble phosphate as precipitating reagent, being led to
Control crystal chemistry plating method is crossed in positive electrode surface one layer of AlPO of uniform plating4Clad, this method is simple to operation, can
Accurate control AlPO4Covering amount, and during cladding by surfactant solve sedimentation problem, make clad Bao Erjun
It is even, improve the cycle life and security performance of positive electrode.
Detailed description of the invention
Fig. 1 is that figure is swept in a kind of face for the nickel-cobalt lithium manganate cathode material EDS that the embodiment of the present invention 1 provides cladding aluminum phosphate.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The embodiment of the present invention provides a kind of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate, chemical expression are as follows:
LiaNixCoyMnzPcO2, wherein 1≤a≤1.2,0.3≤x≤0.98,0.01≤y≤0.6,0.001≤z≤0.2,0.0001
≤c≤0.01。
The doped metallic elements in positive electrode, chemical expression are as follows: LiaNixCoyMnzPcRbO2, wherein b=4/
3-a/3-x-y-z, 0.00001≤b≤0.03, R are metallic element, and metallic element is the period of element other than nickel, cobalt, manganese
One or more combinations of metallic element in table.
The embodiment of the present invention also provides a kind of preparation method of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate, specifically presses
Implement according to following steps:
Step 1, nickel-cobalt lithium manganate cathode material is weighed respectively, measures aluminum salt solution and phosphate solution, wherein nickel cobalt
Nickel in manganate cathode material for lithium, cobalt, manganese the ratio between mole be (0.3-0.98): (0.01-0.6): (0.001-0.1), nickel cobalt manganese
The mass ratio of sour lithium anode material and phosphate solution is 100:(0.01-1), the molar ratio of aluminum salt solution and phosphate solution is
1:(1.1-1.2), the concentration of aluminum salt solution is 0.05mol/L-0.5mol/L, and the concentration of phosphate solution is 0.1mol/L-
1mol/L；
Step 2, the weighed nickel-cobalt lithium manganate cathode material of step 1 is dispersed in water and is heated, wherein nickel cobalt manganese
The mass ratio of sour lithium composite precursor and water is 1:(3-10), the temperature of heating is 30-90 DEG C, obtains nickle cobalt lithium manganate anode slurry
Material；
Step 3, the weighed aluminum salt solution of step 1 and phosphate solution cocurrent are added to the nickle cobalt lithium manganate of step 2
It in anode sizing agent and stirs, while surfactant is added, obtain nickle cobalt lithium manganate slurry, wherein mixing speed 50-200r/
Min, the additive amount of surfactant are the 0.01%-1% of nickle cobalt lithium manganate anode sizing agent quality；
Step 4, by the nickle cobalt lithium manganate slurries filtration of step 3,300-700 DEG C at a temperature of be heat-treated 1-10h to get
Coat the nickel-cobalt lithium manganate cathode material of aluminum phosphate.
The present invention is by, for the source Al, using soluble phosphate as precipitating reagent, passing through control crystal chemistry with aluminum soluble salt
Plating method is in positive electrode surface one layer of AlPO of uniform plating4Clad, this method is simple to operation, accurately controls AlPO4Packet
The amount of covering, and sedimentation problem is solved by surfactant during cladding, keep clad uniform and thin, improves positive electrode
Cycle life and security performance.
Embodiment 1
A kind of preparation method for the nickel-cobalt lithium manganate cathode material coating aluminum phosphate, is specifically implemented according to the following steps:
The nickle cobalt lithium manganate of 1000g nickel cobalt manganese molar ratio 80:15:5 is added in 3000g water, with the speed of 50r/min
Degree is sufficiently stirred, by AlPO4Covering amount is 0.5%, Al:PO4 3-=1:1.1 the concentration of cocurrent addition simultaneously is respectively 0.05mol/L
With the aluminum sulfate and ammonium dihydrogen phosphate of 0.1mol/L, and guarantee to add in 0.5h, filter, it is dry, in air atmosphere
450 DEG C of heat treatment 5h obtain the nickel-cobalt lithium manganate cathode material of MnPO4 cladding.
It is anode with above-mentioned material, metal lithium sheet is that cathode assembles button cell progress charge and discharge contrast test, using this
The positive electrode that inventive method obtains first discharge specific capacity under 1C multiplying power reaches 185mAh/g, holds after 300 charge-discharge cycles
Conservation rate 98.8% is measured, and uncoated positive electrode first discharge specific capacity is 189mAh/g, capacity after 300 charge-discharge cycles
Conservation rate 97.4%.
Embodiment 2
A kind of preparation method for the nickel-cobalt lithium manganate cathode material coating aluminum phosphate, is specifically implemented according to the following steps:
The nickle cobalt lithium manganate of 1000g nickel cobalt manganese molar ratio 80:10:10 is added in 5000g water, with the speed of 50r/min
Degree is sufficiently stirred, by AlPO4Covering amount is 0.1%, Al:PO4 3-Cocurrent addition concentration is respectively==1:1.1 simultaneously
The aluminum sulfate and ammonium dihydrogen phosphate of 0.05mol/L and 0.1mol/L, and guarantee to add in 1.5h, it filters, it is dry, in sky
480 DEG C of heat treatment 5h in gas atmosphere obtain the nickel-cobalt lithium manganate cathode material of MnPO4 cladding.
It is anode with above-mentioned material, metal lithium sheet is that cathode assembles button cell progress charge and discharge contrast test, using this
The positive electrode that inventive method obtains first discharge specific capacity under 1C multiplying power reaches 183mAh/g, holds after 300 charge-discharge cycles
Conservation rate 98.9% is measured, and uncoated positive electrode first discharge specific capacity is 186mAh/g, capacity after 300 charge-discharge cycles
Conservation rate 96.8%.
Embodiment 3
A kind of preparation method for the nickel-cobalt lithium manganate cathode material coating aluminum phosphate, is specifically implemented according to the following steps:
The nickle cobalt lithium manganate of 1000g nickel cobalt manganese molar ratio 85:10:5 is added in 6000g water, with the speed of 50r/min
Degree is sufficiently stirred, by AlPO4Covering amount is 0.2%, Al:PO4 3-Cocurrent addition concentration is respectively==1:1.1 simultaneously
The aluminum sulfate and ammonium dihydrogen phosphate of 0.05mol/L and 0.1mol/L, and guarantee to add in 1.5h, it filters, it is dry, in sky
455 DEG C of heat treatment 4h in gas atmosphere obtain the nickel-cobalt lithium manganate cathode material of MnPO4 cladding.
It is anode with above-mentioned material, metal lithium sheet is that cathode assembles button cell progress charge and discharge contrast test, using this
The positive electrode that inventive method obtains first discharge specific capacity under 1C multiplying power reaches 184mAh/g, holds after 300 charge-discharge cycles
Conservation rate 98.9% is measured, and uncoated positive electrode first discharge specific capacity is 187mAh/g, capacity after 300 charge-discharge cycles
Conservation rate 96.4%.
Fig. 1 is that figure, Cong Tuzhong are swept in a kind of face for the nickel-cobalt lithium manganate cathode material EDS that embodiment 1 provides cladding aluminum phosphate
As can be seen that Al Elemental redistribution is uniform, there is not local over-concentration or local the phenomenon that there is no Al elements.
The present invention is by, for the source Al, using soluble phosphate as precipitating reagent, passing through control crystal chemistry with aluminum soluble salt
Plating method is in positive electrode surface one layer of AlPO of uniform plating4Clad, this method is simple to operation, accurately controls AlPO4Packet
The amount of covering, and sedimentation problem is solved by surfactant during cladding, keep clad uniform and thin, improves positive electrode
Cycle life and security performance.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate, which is characterized in that its chemical expression are as follows:
LiaNixCoyMnzPcO2, wherein 1≤a≤1.2,0.3≤x≤0.98,0.01≤y≤0.6,0.001≤z≤0.2,0.0001
≤c≤0.01。
2. a kind of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate according to claim 1, which is characterized in that in anode
Doped metallic elements in material, chemical expression are as follows: LiaNixCoyMnzPcRbO2, wherein b=4/3-a/3-x-y-z,
0.00001≤b≤0.03, R are metallic element, and the metallic element is metal in the periodic table of elements other than nickel, cobalt, manganese
One or more combinations of element.
3. a kind of preparation method for the nickel-cobalt lithium manganate cathode material for coating aluminum phosphate, which is characterized in that specifically according to following step
It is rapid to implement:
Step 1, nickel-cobalt lithium manganate cathode material is weighed respectively, measures aluminum salt solution and phosphate solution；
Step 2, the weighed nickel-cobalt lithium manganate cathode material of the step 1 is dispersed in water, and is heated, obtain nickel cobalt mangaic acid
Lithium anode sizing agent；
Step 3, aluminum salt solution and phosphate solution that the step 1 measures are added to step according to certain speed cocurrent
It in 2 nickle cobalt lithium manganate slurry and stirs, while surfactant is added；
Step 4, after the completion of charging by the nickle cobalt lithium manganate slurries filtration of the step 3, drying, be heat-treated up to cladding aluminum phosphate
Nickel-cobalt lithium manganate cathode material.
4. a kind of preparation method of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate according to claim 3, feature
Be, nickel in nickel-cobalt lithium manganate cathode material in the step 1, cobalt, manganese the ratio between mole be (0.3-0.98): (0.01-
0.6):(0.001-0.1)。
5. a kind of preparation method of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate according to claim 4, feature
It is, the mass ratio of nickel-cobalt lithium manganate cathode material and phosphate solution is 100:(0.01-1 in the step 1), aluminum salt solution
Molar ratio with phosphate solution is 1:(1.1-1.2).
6. a kind of preparation method of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate according to claim 5, feature
It is, the concentration of aluminum salt solution is 0.05mol/L-0.5mol/L in the step 1, and the concentration of the phosphate solution is
0.1mol/L-1mol/L。
7. a kind of preparation method of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate according to claim 6, feature
It is, the mass ratio of nickel-cobalt lithium manganate cathode material and water is 1:(3-10 in the step 2), the temperature of heating is 30-90 DEG C.
8. a kind of preparation method of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate according to claim 7, feature
It is, mixing speed is 50-200r/min in the step 3.
9. a kind of preparation method of nickel-cobalt lithium manganate cathode material for coating aluminum phosphate according to claim 8, feature
It is, the additive amount of surfactant is the 0.01%-1% of nickle cobalt lithium manganate anode sizing agent quality in the step 3.
10. according to a kind of described in any item preparation sides for the nickel-cobalt lithium manganate cathode material for coating aluminum phosphate claim 3-9
Method, which is characterized in that in the step 4 300-700 DEG C at a temperature of be heat-treated 1-10h.
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