CN113845151B - Cobalt-free ternary positive electrode material and preparation method thereof - Google Patents
Cobalt-free ternary positive electrode material and preparation method thereof Download PDFInfo
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- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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Abstract
The invention discloses a cobalt-free ternary positive electrode material and a preparation method thereof, which relate to the technical field of lithium ion batteries and comprise the following steps: mixing soluble aluminum salt and soluble nickel salt, and adding the mixture into pure water to prepare aluminum-nickel inorganic salt mixed solution; taking an aluminum-nickel inorganic salt mixed solution, an ammonia water solution and a sodium hydroxide solution as raw materials for coprecipitation reaction, aging after the reaction is completed, and then filtering, washing and drying to obtain an aluminum-nickel precursor; adding the aluminum nickel precursor into a potassium permanganate solution, stirring, then carrying out microwave treatment, cooling, washing and drying to obtain an aluminum nickel manganese precursor; mixing the aluminum nickel manganese precursor and lithium salt, sintering in air or oxygen atmosphere, cooling and grinding. The cobalt-free ternary positive electrode material prepared by the method has the advantages that the cost of the material is greatly reduced because the cobalt-free ternary positive electrode material does not contain Co element, the stability of the material is improved due to the introduction of Al and Mn elements, and compared with the cobalt-containing ternary positive electrode material NCM, the cycle performance of the cobalt-free ternary positive electrode material has no obvious difference.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a cobalt-free ternary positive electrode material and a preparation method thereof.
Background
Lithium ion batteries are energy storage devices with high energy density and high efficiency, and are widely applied to the fields of portable digital equipment, electric automobiles and the like at present. The lithium ion battery system is composed of four key materials, namely a positive electrode material, a negative electrode material, a diaphragm and electrolyte, so that the properties of the materials are directly related to the performance of the lithium ion battery.
In the recent stage, which is the golden period of new energy power automobile development, the main current positive electrode materials of the power lithium ion battery for the automobile comprise lithium iron phosphate and ternary materials, and the ternary materials are widely paid attention to by people due to higher energy density. Common ternary materials comprise nickel cobalt lithium manganate, nickel cobalt lithium aluminate and the like, and the common ternary materials can be seen to contain cobalt, compared with nickel and manganese, the price of cobalt is high, the storage capacity is low, and therefore the ternary materials have no cobalt or low cobalt and are considered.
The cobalt-free ternary cathode materials containing nickel, manganese and other elements are generally prepared by adopting a coprecipitation method, and manganese salt, nickel salt and the like are subjected to coprecipitation reaction with ammonia water and sodium hydroxide solution. However, the difficulty of preparing the cobalt-free ternary cathode material by the coprecipitation method is high, and three elements cannot be precipitated uniformly together, so that the material cannot reach the required performance.
Disclosure of Invention
Based on the technical problems in the background technology, the invention provides a cobalt-free ternary positive electrode material and a preparation method thereof, wherein an aluminum-nickel binary precursor is prepared by adopting a coprecipitation method, and then the precursor is subjected to microwave reaction in a potassium permanganate solution to obtain an aluminum-nickel manganese ternary precursor, so that the cobalt-free ternary positive electrode material has excellent electrochemical performance.
The invention provides a preparation method of a cobalt-free ternary positive electrode material, which comprises the following steps:
s1, mixing soluble aluminum salt and soluble nickel salt, and adding the mixture into pure water to prepare aluminum-nickel inorganic salt mixed solution;
s2, performing coprecipitation reaction by taking an aluminum-nickel inorganic salt mixed solution, an ammonia water solution and a sodium hydroxide solution as raw materials, aging after the reaction is completed, and filtering, washing and drying to obtain an aluminum-nickel precursor;
s3, adding the aluminum nickel precursor into a potassium permanganate solution, stirring, then carrying out microwave treatment, cooling, washing and drying to obtain an aluminum nickel manganese precursor;
s4, mixing the aluminum nickel manganese precursor and lithium salt, sintering in an air atmosphere or an oxygen atmosphere, cooling and grinding to obtain the aluminum nickel manganese alloy.
Preferably, the chemical formula of the cobalt-free ternary positive electrode material satisfies: liNi x Al y Mn z O 2 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x+y+z=1, x: y: z=4-8: 0.5-3:0.5-3.
Preferably, the specific operation of the microwave treatment is: the microwave power is 200-1000W, after each microwave treatment for 10-60s, the microwave treatment is repeated for 2-10 times after cooling to room temperature.
Preferably, in S2, the specific operation of the coprecipitation reaction is as follows: adding ammonia water solution into a reaction container, regulating the pH value of the reaction system, then simultaneously dripping the aluminum nickel inorganic salt solution, the ammonia water solution and the sodium hydroxide solution into the reaction container, and controlling the pH value of the reaction system by regulating the dripping speeds of the ammonia water solution and the sodium hydroxide solution.
Preferably, the concentration of the aqueous ammonia solution is 0.1 to 5mol/L.
Preferably, the pH of the reaction system of the coprecipitation reaction is controlled to 7-13.
Preferably, in S2, the ageing is carried out for 4-12 hours.
Preferably, in S4, the molar ratio of the aluminum nickel manganese precursor to the lithium salt is 1:1 to 1.5; the lithium salt is at least one of lithium carbonate, lithium hydroxide and lithium nitrate.
Preferably, the sintering is performed by presintering for 4-12h at 450-650 ℃, and then heating to 800-950 ℃ for sintering for 8-36h.
The invention also provides the cobalt-free ternary anode material prepared by the method.
The cobalt-free ternary positive electrode material can be used as a positive electrode active material for a lithium ion battery.
The beneficial effects are that: the invention provides a preparation method of a cobalt-free ternary cathode material, which comprises the steps of preparing an aluminum-nickel binary precursor by adopting a coprecipitation method, and then carrying out microwave reaction on the precursor in a potassium permanganate solution to obtain an aluminum-nickel manganese ternary precursor; compared with the defect that the co-precipitation method adopted to prepare the ternary precursor cannot achieve co-uniform precipitation in the prior art, the method adopts the binary co-precipitation method and then carries out microwave reaction to introduce another element, so that the uniformity of three elements in the product is higher, and the material performance is not inferior to that of the cobalt-containing ternary material. The cobalt-free ternary positive electrode material prepared by the method provided by the invention does not contain Co element, so that the material cost is greatly reduced, the stability of the material is improved due to the introduction of Al and Mn elements, and the cycle performance is not obviously different from that of the ternary positive electrode material NCM.
Drawings
FIG. 1 shows a cobalt-free ternary cathode material LiNi prepared in example 1 of the present invention 0.8 Al 0.1 Mn 0.1 O 2 (NAM)Ternary cathode material LiNi of comparative example 0.8 Co 0.1 Mn 0.1 O 2 (NCM) cycle performance chart.
Detailed Description
The technical scheme of the invention is described in detail through specific embodiments.
Example 1
A cobalt-free ternary positive electrode material has a chemical formula: liNi 0.8 Al 0.1 Mn 0.1 O 2 The method comprises the steps of carrying out a first treatment on the surface of the The preparation method comprises the following steps:
s1, sodium metaaluminate and nickel chloride are processed according to n Al ：n Ni =1: 8, mixing, and adding the mixture into pure water to prepare 2mol/L aluminum nickel inorganic salt mixed solution;
s2, performing coprecipitation reaction by taking aluminum-nickel inorganic salt mixed solution, 2mol/L ammonia water solution and sodium hydroxide solution as raw materials, wherein the specific operation is as follows: adding ammonia water solution into a reaction container, regulating the pH value of a reaction system, then simultaneously dropwise adding an aluminum nickel inorganic salt solution, the ammonia water solution and a sodium hydroxide solution into the reaction container, and controlling the pH value range of the reaction system to be 9.5 by regulating the dropwise adding speed of the ammonia water solution and the sodium hydroxide solution; aging for 8 hours after the reaction is completed, and filtering, washing and drying to obtain an aluminum-nickel precursor;
s3, adding the aluminum nickel precursor into a 3mol/L potassium permanganate solution, stirring, and then carrying out microwave treatment, wherein the specific operation is as follows: the microwave power is 500W, the microwave is cooled to the room temperature after 30 seconds of each microwave treatment, and then the microwave treatment-cooling step is repeated for 3 times; cooling to room temperature, washing and drying to obtain an aluminum nickel manganese precursor;
s4, mixing the aluminum nickel manganese precursor and lithium hydroxide according to the following ratio of 1: mixing at a molar ratio of 1.15, presintering at 500 ℃ for 6 hours in an oxygen atmosphere, heating to 850 ℃ and sintering for 24 hours, cooling and grinding to obtain the composite material.
Example 2
A cobalt-free ternary positive electrode material has a chemical formula: liNi 0.7 Al 0.15 Mn 0.15 O 2 The method comprises the steps of carrying out a first treatment on the surface of the The preparation method comprises the following steps:
s1, sodium metaaluminate and chlorineNickel sulfide according to n Al ：n Ni =1.5: 7, mixing, and adding the mixture into pure water to prepare 2mol/L aluminum nickel inorganic salt mixed solution;
s2, performing coprecipitation reaction by taking aluminum-nickel inorganic salt mixed solution, 2mol/L ammonia water solution and sodium hydroxide solution as raw materials, wherein the specific operation is as follows: adding ammonia water solution into a reaction container, regulating the pH value of a reaction system, then simultaneously dropwise adding an aluminum nickel inorganic salt solution, the ammonia water solution and a sodium hydroxide solution into the reaction container, and controlling the pH value range of the reaction system to be 9.5 by regulating the dropwise adding speed of the ammonia water solution and the sodium hydroxide solution; aging for 8 hours after the reaction is completed, and filtering, washing and drying to obtain an aluminum-nickel precursor;
s3, adding the aluminum nickel precursor into a 3mol/L potassium permanganate solution, stirring, and then carrying out microwave treatment, wherein the specific operation is as follows: the microwave power is 800W, after each microwave treatment for 40s, the temperature is cooled to the room temperature, and then the microwave treatment-cooling step is repeated for 4 times; cooling to room temperature, washing and drying to obtain an aluminum nickel manganese precursor;
s4, mixing the aluminum nickel manganese precursor and lithium hydroxide according to the following ratio of 1: mixing at a molar ratio of 1.15, presintering at 500 ℃ for 6h in an air atmosphere or an oxygen atmosphere, heating to 850 ℃ and sintering for 24h, cooling and grinding to obtain the composite material.
Example 3
A cobalt-free ternary positive electrode material has a chemical formula: liNi 0.8 Al 0.05 Mn 0.15 O 2 The method comprises the steps of carrying out a first treatment on the surface of the The preparation method comprises the following steps:
s1, sodium metaaluminate and nickel chloride are processed according to n Al ：n Ni =0.5: 8, mixing, and adding the mixture into pure water to prepare 2mol/L aluminum nickel inorganic salt mixed solution;
s2, performing coprecipitation reaction by taking aluminum-nickel inorganic salt mixed solution, 2mol/L ammonia water solution and sodium hydroxide solution as raw materials, wherein the specific operation is as follows: adding ammonia water solution into a reaction container, regulating the pH value of a reaction system, then simultaneously dropwise adding an aluminum nickel inorganic salt solution, the ammonia water solution and a sodium hydroxide solution into the reaction container, and controlling the pH value range of the reaction system to be 9.5 by regulating the dropwise adding speed of the ammonia water solution and the sodium hydroxide solution; aging for 8 hours after the reaction is completed, and filtering, washing and drying to obtain an aluminum-nickel precursor;
s3, adding the aluminum nickel precursor into a 3mol/L potassium permanganate solution, stirring, and then carrying out microwave treatment, wherein the specific operation is as follows: the microwave power is 800W, after each microwave treatment for 40s, the temperature is cooled to the room temperature, and then the microwave treatment-cooling step is repeated for 4 times; cooling to room temperature, washing and drying to obtain an aluminum nickel manganese precursor;
s4, mixing the aluminum nickel manganese precursor and lithium hydroxide according to the following ratio of 1: mixing at a molar ratio of 1.15, presintering at 500 ℃ for 6 hours in an oxygen atmosphere, heating to 850 ℃ and sintering for 24 hours, cooling and grinding to obtain the composite material.
Example 4
A cobalt-free ternary positive electrode material has a chemical formula: liNi 0.8 Al 0.15 Mn 0.05 O 2 The method comprises the steps of carrying out a first treatment on the surface of the The preparation method comprises the following steps:
s1, sodium metaaluminate and nickel chloride are processed according to n Al ：n Ni =1.5: 8, mixing, and adding the mixture into pure water to prepare 2mol/L aluminum nickel inorganic salt mixed solution;
s2, performing coprecipitation reaction by taking aluminum-nickel inorganic salt mixed solution, 2mol/L ammonia water solution and sodium hydroxide solution as raw materials, wherein the specific operation is as follows: adding ammonia water solution into a reaction container, regulating the pH value of a reaction system, then simultaneously dropwise adding an aluminum nickel inorganic salt solution, the ammonia water solution and a sodium hydroxide solution into the reaction container, and controlling the pH value range of the reaction system to be 9.5 by regulating the dropwise adding speed of the ammonia water solution and the sodium hydroxide solution; aging for 8 hours after the reaction is completed, and filtering, washing and drying to obtain an aluminum-nickel precursor;
s3, adding the aluminum nickel precursor into a 3mol/L potassium permanganate solution, stirring, and then carrying out microwave treatment, wherein the specific operation is as follows: the microwave power is 400W, the microwave is cooled to room temperature after 20s of each microwave treatment, and then the microwave treatment-cooling step is repeated for 2 times; cooling to room temperature, washing and drying to obtain an aluminum nickel manganese precursor;
s4, mixing the aluminum nickel manganese precursor and lithium hydroxide according to the following ratio of 1: mixing at a molar ratio of 1.15, presintering at 500 ℃ for 6 hours in an oxygen atmosphere, heating to 850 ℃ and sintering for 24 hours, cooling and grinding to obtain the composite material.
The cobalt-free ternary cathode materials (NAM) prepared in the examples 1 to 4 of the present invention were used as cathode active materials, respectively, for preparing lithium ion batteries, and further testing the performance thereof; and adopts ternary anode material LiNi 0.8 Co 0.1 Mn 0.1 O 2 (NCM, commercially available) was compared as a comparative example.
The method comprises the following specific steps:
1. preparing a positive electrode of a lithium ion battery: mixing 80 parts of positive electrode active material and 10 parts of conductive agent acetylene black, grinding, then adding 10 parts of binder PVDF, stirring and mixing, and mixing to obtain positive electrode slurry; coating the positive electrode slurry on a metal current collector (Al foil) to form a coating layer with the thickness of 10-200 mu m, and vacuum drying the coating layer in an oven at 80 ℃ for 12-24 hours to remove the solvent to obtain the positive electrode.
2. And (3) battery assembly: the anode prepared by the method has a lithium sheet as a negative electrode, a celgard2400 as a diaphragm and LiPF as an electrolyte 6 The DEC/EC/EMC is assembled into a button cell;
3. performance test:
a. gram capacity test;
capacity retention after 100 cycles;
c. cycle performance at 3.0-4.3V voltage.
4. Test results: see table 1 and fig. 1.
TABLE 1 Performance test results
| Performance index | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| Gram capacity mAh/g | 185.3 | 173.5 | 184.3 | 184.7 | 186.8 |
| Capacity retention% | 95.3 | 95.8 | 95.1 | 95.6 | 95.5 |
As can be seen from Table 1 and FIG. 1, the cobalt-free ternary cathode material prepared by the invention is compared with the conventional cobalt-containing ternary cathode material LiNi 0.8 Co 0.1 Mn 0.1 O 2 There was no significant difference in performance.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (6)
1. The preparation method of the cobalt-free ternary positive electrode material is characterized by comprising the following steps of:
s1, mixing soluble aluminum salt and soluble nickel salt, and adding the mixture into pure water to prepare aluminum-nickel inorganic salt mixed solution;
s2, adding an ammonia water solution into a reaction container, adjusting the pH value of a reaction system, then dropwise adding an aluminum-nickel inorganic salt solution, the ammonia water solution and a sodium hydroxide solution into the reaction container at the same time, controlling the pH value of the reaction system by adjusting the dropwise adding speed of the ammonia water solution and the sodium hydroxide solution, controlling the pH range of the reaction system in a coprecipitation reaction to be 9.5, aging after the reaction is completed, and then filtering, washing and drying to obtain an aluminum-nickel precursor;
s3, adding the aluminum nickel precursor into a potassium permanganate solution, stirring, then carrying out microwave treatment, cooling, washing and drying to obtain an aluminum nickel manganese precursor; the microwave power is 200-1000W, after each microwave treatment for 10-60s, the microwave treatment is repeated for 2-10 times after cooling to room temperature;
s4, mixing the aluminum nickel manganese precursor and lithium salt, sintering in an air atmosphere or an oxygen atmosphere, cooling and grinding to obtain the aluminum nickel manganese precursor;
the chemical formula of the cobalt-free ternary positive electrode material is as follows: liNi x Al y Mn z O 2 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x+y+z=1, x: y: z=4-8: 0.5-3:0.5-3.
2. The method for preparing a cobalt-free ternary cathode material according to claim 1, wherein the concentration of the aqueous ammonia solution is 0.1-5mol/L.
3. The method for preparing a cobalt-free ternary cathode material according to claim 1, wherein in S2, aging is performed for 4-12 hours.
4. The method for preparing a cobalt-free ternary cathode material according to claim 1, wherein in S4, the molar ratio of the aluminum nickel manganese precursor to the lithium salt is 1:1 to 1.5; the lithium salt is at least one of lithium carbonate, lithium hydroxide and lithium nitrate.
5. The method for preparing the cobalt-free ternary cathode material according to claim 1, wherein the sintering is performed by presintering for 4-12h at 450-650 ℃, then heating to 800-950 ℃ and sintering for 8-36h.
6. A cobalt-free ternary positive electrode material prepared by the method of any one of claims 1-5.
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