CN109301196B - Method for coating lithium nickel cobalt manganese oxide positive electrode material with lithium manganese phosphate - Google Patents
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
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- 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
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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
- H01M4/58—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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- 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 relates to the technical field of lithium battery anode materials, in particular to a method for coating a lithium nickel cobalt manganese oxide anode material with lithium manganese phosphate.
Description
Technical Field
The invention relates to the technical field of lithium battery positive electrode materials, in particular to a method for coating a nickel cobalt lithium manganate positive electrode material with lithium manganese phosphate.
Background
With the increasing emphasis on energy and environmental issues, lithium ion batteries are gaining favor of many consumers as one of clean and efficient energy storage and conversion media. Lithium ion batteries are widely used in portable mobile devices such as mobile phones, notebook computers, cameras, and the like.
Currently, commercial lithium ion battery positive electrode materials mainly include lithium cobaltate, lithium manganate, lithium iron phosphate, lithium nickel cobalt manganese oxide and the like, wherein the lithium cobaltate has high cost, and potential safety hazards exist during overcharge; the layered lithium manganate has poor structural stability, the spinel lithium manganate has low specific capacity, and the structural stability at high temperature needs to be improved. The lithium iron phosphate has poor processing performance, low tap density and low energy density; compared with the prior art, the nickel cobalt lithium manganate material has the advantages of low cost, good high-temperature performance, high energy density, excellent processing performance and the like, and is widely used. However, in the using process, the high rate performance and the cycling stability of the nickel cobalt lithium manganate material are found to be poorer than those of lithium cobaltate, and the surface of the nickel cobalt lithium manganate material needs to be modified to improve the electrochemical performance of the nickel cobalt lithium manganate material. At present, carbon is adopted to coat nickel cobalt lithium manganate, and after coating, the rate capability and the cycling stability of the anode material are improved. And calcium fluophosphate is adopted to coat the nickel cobalt lithium manganate, so that the cycling stability is improved. In addition, lithium manganese phosphate is adopted to coat the lithium nickel cobalt manganese oxide positive electrode material, for example, the patent number is 201510365733.X, so that the purposes of reducing cost, easily popularizing and improving the cycling stability and rate capability of the lithium nickel cobalt manganese oxide are achieved.
However, continuous optimization of material performance is a direction in which technicians in the field continuously pursue and research and develop, and can further improve and perfect the performance of the lithium nickel cobalt manganese oxide positive electrode material, so that the process for improving the lithium nickel cobalt manganese oxide positive electrode material is further optimized and perfected, the performance improvement cost is reduced, and the electrochemical performance is enhanced, which becomes a key and key technical problem in current research.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a method for coating a lithium manganese phosphate on a lithium nickel cobalt manganese oxide positive electrode material.
The method is realized by the following technical scheme:
the method for coating the lithium nickel cobalt manganese oxide positive electrode material with the lithium manganese phosphate comprises the following steps of:
(1) mixing phosphoric acid and urea according to the ratio of 2:0.7-1.1, and heating to 80-100 ℃ for reaction to generate a mixture containing urea phosphate; mixing lithium carbonate and manganese nitrate according to the mass ratio of 1:1, adding the mixture into a urea phosphate-containing mixture, uniformly stirring the mixture, adding water to prepare a solution, and adjusting the pH value to 3.8-4.1, wherein the addition accounts for 20-40% of the urea phosphate-containing mixture;
(2) adding solid powder of nickel cobalt lithium manganate into the solution obtained in the step (1), wherein the adding amount is 60-80% (w/v);
(3) stirring and evaporating the mixed material in the step (2) at the temperature of 100-120 ℃ until the solution is concentrated to be viscous, ageing at normal temperature for 5-8h, drying at the temperature of 50-70 ℃ for 4-5h, carrying out jet milling, and sieving with a 400-mesh sieve;
(4) and (4) roasting the powder in the step (3) at the temperature of 600-.
Preferably, the jet milling pressure is 0.4-0.5 MPa.
Preferably, in the step (3), the drying temperature is 60 ℃.
Preferably, in the step (4), the roasting temperature is 700 ℃.
Preferably, in the step (1), phosphoric acid and urea are mixed according to a ratio of 2:1.
Preferably, the manganese nitrate is replaced by manganese acetate.
Compared with the prior art, the invention has the technical effects that:
the phosphoric acid and the urea are mixed according to a certain proportion, and the temperature rise reaction is carried out, so that not only is the phosphorus source required to be added guaranteed, but also a urea phosphate structure with a certain complexing function can be formed, the lithium source and the manganese source are added without adding other complexing agents, after the lithium source and the manganese source are added, the manganese lithium phosphate component is formed through urea phosphate complexing precipitation, and the nickel cobalt lithium manganate is coated by combining the addition of the nickel cobalt lithium manganate component, so that the electrochemical performance of the nickel cobalt lithium manganate anode material is improved, the raw material cost is reduced, and the process flow is shortened.
The invention particularly carries out coating treatment under the action of phosphoric acid and urea, so that the cycle electrochemical performance of the prepared nickel cobalt lithium manganate cathode material is improved, and the attenuation rate of cycle discharge capacity is reduced.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
The nickel cobalt lithium manganate material adopted in the following examples is: LiNi0.5Mn0.3Co0.2O2。
Example 1
The method for coating the lithium nickel cobalt manganese oxide positive electrode material with the lithium manganese phosphate comprises the following steps of:
(1) mixing phosphoric acid and urea according to the ratio of 2:0.7, and heating to 80 ℃ to react to generate a mixture containing urea phosphate; mixing lithium carbonate and manganese nitrate according to the mass ratio of 1:1, adding the mixture into a urea phosphate-containing mixture, uniformly stirring the mixture, adding water to prepare a solution, and adjusting the pH value to 3.8, wherein the addition accounts for 20% of the urea phosphate-containing mixture;
(2) adding solid powder of nickel cobalt lithium manganate into the solution in the step (1), wherein the adding amount is 60% (w/v);
(3) stirring and evaporating the mixed material in the step (2) at 100 ℃ until the solution is concentrated to be viscous, ageing at normal temperature for 5h, drying at 50 ℃ for 4h, carrying out jet milling under the pressure of 0.4MPa, and sieving by a 400-mesh sieve;
(4) and (4) roasting the powder obtained in the step (3) at 600 ℃ for 4h, and cooling to normal temperature.
Example 2
The method for coating the lithium nickel cobalt manganese oxide positive electrode material with the lithium manganese phosphate comprises the following steps of:
(1) mixing phosphoric acid and urea according to the ratio of 2:1.1, and heating to 100 ℃ to react to generate a mixture containing urea phosphate; mixing lithium carbonate and manganese nitrate according to the mass ratio of 1:1, adding the mixture into a urea phosphate-containing mixture, uniformly stirring the mixture, adding water to prepare a solution, and adjusting the pH value to 4.1, wherein the addition accounts for 40% of the urea phosphate-containing mixture;
(2) adding solid powder of nickel cobalt lithium manganate into the solution in the step (1), wherein the adding amount is 80% (w/v);
(3) stirring and evaporating the mixed material in the step (2) at 120 ℃ until the solution is concentrated to be viscous, ageing at normal temperature for 8h, drying at 70 ℃ for 5h, carrying out jet milling under the pressure of 0.5MPa, and sieving by a 400-mesh sieve;
(4) and (4) roasting the powder obtained in the step (3) at 800 ℃ for 5 hours, and cooling to normal temperature to obtain the catalyst.
Example 3
The method for coating the lithium nickel cobalt manganese oxide positive electrode material with the lithium manganese phosphate comprises the following steps of:
(1) mixing phosphoric acid and urea according to the ratio of 2:1, and heating to 90 ℃ to react to generate a mixture containing urea phosphate; mixing lithium carbonate and manganese nitrate according to the mass ratio of 1:1, adding the mixture into a urea phosphate-containing mixture, uniformly stirring the mixture, adding water to prepare a solution, and adjusting the pH value to be 4, wherein the addition amount of the solution accounts for 30% of the urea phosphate-containing mixture;
(2) adding solid powder of nickel cobalt lithium manganate into the solution in the step (1), wherein the adding amount is 70% (w/v);
(3) stirring and evaporating the mixed material in the step (2) at 110 ℃ until the solution is concentrated to be viscous, ageing for 7h at normal temperature, drying for 4.5h at 60 ℃, carrying out jet milling under the pressure of 0.45MPa, and sieving by a 400-mesh sieve;
(4) and (4) roasting the powder obtained in the step (3) at 700 ℃ for 4h, and cooling to normal temperature to obtain the catalyst.
Example 4
The method for coating the lithium nickel cobalt manganese oxide positive electrode material with the lithium manganese phosphate comprises the following steps of:
(1) mixing phosphoric acid and urea according to the ratio of 2:1.1, and heating to 80 ℃ to react to generate a mixture containing urea phosphate; mixing lithium carbonate and manganese nitrate according to the mass ratio of 1:1, adding the mixture into a urea phosphate-containing mixture, uniformly stirring the mixture, adding water to prepare a solution, and adjusting the pH value to 3.9, wherein the addition accounts for 25% of the urea phosphate-containing mixture;
(2) adding solid powder of nickel cobalt lithium manganate into the solution in the step (1), wherein the adding amount is 80% (w/v);
(3) stirring and evaporating the mixed material in the step (2) at 100 ℃ until the solution is concentrated to be viscous, ageing at normal temperature for 7h, drying at 50 ℃ for 5h, carrying out jet milling under the pressure of 0.5MPa, and sieving by a 400-mesh sieve;
(4) and (4) roasting the powder obtained in the step (3) at 800 ℃ for 4.5h, and cooling to normal temperature to obtain the catalyst.
Example 5
In contrast to example 1, manganese nitrate was used instead of manganese acetate.
Example 6
In contrast to example 1, manganese nitrate was used instead of manganese sulfate.
Example 7
In contrast to example 1, the phosphoric acid used was potassium dihydrogen phosphate instead.
The lithium manganese phosphate coated lithium nickel cobalt manganese oxide material prepared in examples 1 to 7 is used as a positive electrode material, a metal lithium sheet is used as a negative electrode material, a button cell is assembled, and the battery is subjected to cyclic discharge for 200 times under the voltage of 2.5 to 3V and the multiplying power of 1C, and the capacity retention rate is detected, and the results are shown in the following table 1:
TABLE 1
| First discharge capacity (mAh/g) | 200 discharge capacity (mAh/g) | Capacity retention (%) | |
| Example 1 | 172.8 | 164.5 | 4.80 |
| Example 2 | 175.4 | 168.1 | 4.16 |
| Example 3 | 174.6 | 167.3 | 4.18 |
| Example 4 | 173.5 | 166.9 | 3.80 |
| Example 5 | 178.4 | 168.7 | 5.44 |
| Example 6 | 147.9 | 108.5 | 26.64 |
| Example 7 | 151.6 | 109.4 | 27.84 |
| Control (LiNi)0.5Mn0.3Co0.2O2） | 150.7 | 104.8 | 30.46 |
The data in table 1 show that, after phosphoric acid and urea are used in the invention, the phosphoric acid and urea are used as phosphorus sources to be mixed with lithium sources and manganese sources, and the mixture is coated after lithium nickel cobalt manganese oxide powder is added, so that the lithium manganese phosphate coats the lithium nickel cobalt manganese oxide material, the electrochemical performance of the cathode material is effectively improved, the stability of the electrochemical performance is greatly enhanced, and the capacity attenuation rate in the charging and discharging process is reduced.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. The method for coating the lithium nickel cobalt manganese oxide positive electrode material with the lithium manganese phosphate is characterized by comprising the following steps of:
(1) mixing phosphoric acid and urea according to the ratio of 2:0.7-1.1, and heating to 80-100 ℃ for reaction to generate a mixture containing urea phosphate; mixing lithium carbonate and manganese nitrate according to the mass ratio of 1:1, adding the mixture into a urea phosphate-containing mixture, uniformly stirring the mixture, adding water to prepare a solution, and adjusting the pH value to 3.8-4.1, wherein the addition accounts for 20-40% of the urea phosphate-containing mixture;
(2) adding solid powder of nickel cobalt lithium manganate into the solution obtained in the step (1), wherein the adding amount is 60-80 w/v%;
(3) stirring and evaporating the mixed material in the step (2) at the temperature of 100-120 ℃ until the solution is concentrated to be viscous, aging at normal temperature for 5-8h, drying at the temperature of 50-70 ℃ for 4-5h, carrying out jet milling, and sieving with a 400-mesh sieve;
(4) and (4) roasting the powder in the step (3) at the temperature of 600-.
2. The method for coating the lithium manganese phosphate on the lithium nickel cobalt manganese oxide positive electrode material according to claim 1, wherein the jet milling pressure is 0.4-0.5 MPa.
3. The method for coating lithium manganese phosphate on a lithium nickel cobalt manganese oxide positive electrode material according to claim 1, wherein in the step (3), the drying temperature is 60 ℃.
4. The method for coating lithium manganese phosphate on a lithium nickel cobalt manganese oxide positive electrode material according to claim 1, wherein in the step (4), the roasting temperature is 700 ℃.
5. The method for coating a lithium manganese phosphate on a lithium nickel cobalt manganese oxide positive electrode material according to claim 1, wherein in the step (1), phosphoric acid and urea are mixed according to a ratio of 2:1.
6. The method for coating the lithium manganese phosphate on the lithium nickel cobalt manganese oxide positive electrode material according to claim 1, wherein the manganese nitrate is replaced by manganese acetate.
7. The lithium manganese phosphate coated lithium nickel cobalt manganese oxide positive electrode material prepared by the method of any one of claims 1 to 6.
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