CN111326731A - Preparation method of nickel-cobalt-manganese ternary material and lithium ion battery - Google Patents
Preparation method of nickel-cobalt-manganese ternary material and lithium ion battery Download PDFInfo
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- CN111326731A CN111326731A CN201811542942.7A CN201811542942A CN111326731A CN 111326731 A CN111326731 A CN 111326731A CN 201811542942 A CN201811542942 A CN 201811542942A CN 111326731 A CN111326731 A CN 111326731A
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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
- 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
- H01M4/52—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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a preparation method of a nickel-cobalt-manganese ternary material and a lithium ion battery, which comprises the following steps: adding three materials of nickel hydroxide, cobalt hydroxide and manganese carbonate used as raw materials and lithium carbonate used as a lithium source into deionized water for mixing to obtain a suspension, adding glucose into the suspension, and uniformly stirring to obtain a mixed solution; and pouring the mixed solution into a ball mill for ball milling to obtain ball milling suspension. According to the preparation method of the nickel-cobalt-manganese ternary material and the lithium ion battery, the glucose is added in the preparation process of the ternary material, so that the ternary material with high tap density and good sphericity can be obtained under the conditions that the preparation steps are not increased and the electrochemical performance and the cycle performance of the ternary material are not influenced, the operation process is convenient and simple, the cost is low, the obtained effect is good, and the preparation method is suitable for large-scale popularization and use.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a preparation method of a nickel-cobalt-manganese ternary material and a lithium ion battery.
Background
The anode materials adopted by the existing lithium ion battery mainly comprise lithium cobaltate, lithium iron phosphate, lithium manganate, ternary anode materials and the like. The nickel cobalt lithium manganate ternary positive electrode material has the advantages of high specific capacity, good safety performance and rate discharge performance and the like, is a lithium ion power battery positive electrode material with great potential, and has wide application prospects in the power fields of electric vehicles and ships, electric spacecrafts, electric tools and the like.
The ternary material combines the advantages of the three elements at the same time through the synergistic effect of the three elements of Ni-Co-Mn. For example, the good cycle performance of LiCoO2, the high specific energy of LiNiO2, and the high safety and low cost of LiMnO2 have become one of the most promising new positive electrode materials for lithium ion batteries.
In the prior art, three substances, namely nickel hydroxide, cobalt hydroxide and manganese carbonate, are used as raw materials, ball milling is carried out on the raw materials by using a ball mill, and the ternary material which is formed by calcining after spray drying not only saves the preparation process of a precursor and meets the requirement of cost reduction, but also has no pollution gas generated in the sintering process, and is very environment-friendly. However, the ternary material prepared by the method has low tap density, so that the industrial development process is limited to a certain extent.
The main reason for the above problems is that the particle size of the ternary material after ball milling in the ball mill becomes smaller, and in order to ensure smooth proceeding of the subsequent spray drying process, the solid content of the material must be reduced, so that the tap density of the prepared ternary material is lower.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing a nickel-cobalt-manganese ternary material and a lithium ion battery, so as to solve the problem that the nickel-cobalt-manganese ternary material prepared by using the existing preparation method has a low tap density.
In order to achieve the above purpose, in one aspect, the invention adopts the following technical scheme:
a preparation method of a nickel-cobalt-manganese ternary material comprises the following steps: adding three materials of nickel hydroxide, cobalt hydroxide and manganese carbonate used as raw materials and lithium carbonate used as a lithium source into deionized water for mixing to obtain a suspension,
the preparation method also comprises the following steps:
adding glucose into the suspension and uniformly stirring to obtain a mixed solution;
and pouring the mixed solution into a ball mill for ball milling to obtain ball milling suspension.
Preferably, the mass of the glucose is 1% to 10% of the mass of the raw material.
Preferably, in the ball milling process, the rotation speed of the ball mill is 3000-4000 rpm/min, and the duration of the ball milling process is 3.5-6 hours.
Preferably, the preparation method further comprises the following steps:
and carrying out spray drying on the ball milling suspension to carry out primary particle forming, thus obtaining a mixture.
Preferably, a spray drying apparatus is used in performing the spray drying process,
the inlet temperature of the spray drying equipment is 250 ℃ to 290 ℃; and/or the presence of a gas in the gas,
the air flow of the spray drying equipment is 4m3H to 7m3/h。
Preferably, the particle size of the mix is 1 μm to 20 μm in size.
Preferably, the preparation method further comprises:
and placing the mixture in an atmosphere muffle furnace, carrying out secondary particle forming on the mixture under a preset condition, and naturally cooling to obtain the nickel cobalt lithium manganate capable of being used as a battery anode material.
Preferably, the predetermined condition includes: continuously heating under the air or oxygen atmosphere at a first temperature change value, and raising the temperature in the atmosphere muffle furnace to a first preset temperature for a first preset time;
and continuously heating according to a second temperature change value, and raising the temperature in the atmosphere muffle furnace to a second preset temperature for a second preset time.
Preferably, the first temperature variation value is 8 ℃/min to 12 ℃/min; and/or the presence of a gas in the gas,
the second temperature change value is 18 ℃/min to 22 ℃/min; and/or the presence of a gas in the gas,
the first predetermined temperature is 350 ℃ to 650 ℃; and/or the presence of a gas in the gas,
the second predetermined temperature is 850 ℃ to 1000 ℃; and/or the presence of a gas in the gas,
the first predetermined time period is 4 to 6 hours; and/or the presence of a gas in the gas,
the second predetermined period of time is 10 hours to 16 hours.
In order to achieve the purpose, on the other hand, the invention adopts the following technical scheme:
the lithium ion battery comprises a positive electrode, wherein the positive electrode comprises a ternary material, and the ternary material is prepared by adopting the preparation method of the nickel-cobalt-manganese ternary material.
According to the preparation method of the nickel-cobalt-manganese ternary material and the lithium ion battery, the glucose is added in the preparation process of the ternary material, so that the ternary material with high tap density and good sphericity can be obtained under the conditions that the preparation steps are not increased and the electrochemical performance and the cycle performance of the ternary material are not influenced, the operation process is convenient and simple, the cost is low, the obtained effect is good, and the preparation method is suitable for large-scale popularization and use.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent from the following description of the embodiments of the present invention with reference to the accompanying drawings, in which:
fig. 1 is a graph showing a relationship between tap density and added glucose content of a ternary material prepared by a method for preparing a nickel-cobalt-manganese ternary material according to an embodiment of the present invention;
FIG. 2 shows a graph of the number of cycles of the ternary material versus gram volume when glucose is added in an amount of 3% of the mass of the raw material, provided by an embodiment of the present invention;
FIG. 3 shows an SEM image of a ternary material when glucose is added in an amount of 3% by mass of the raw material provided by an embodiment of the present invention;
fig. 4 shows an SEM image of the ternary material without added glucose.
Detailed Description
The present invention is described below based on embodiments, and it will be understood by those of ordinary skill in the art that the drawings provided herein are for illustrative purposes and are not necessarily drawn to scale.
Unless the context clearly requires otherwise, throughout the description and the claims, the words "comprise", "comprising", and the like are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense; that is, what is meant is "including, but not limited to".
The application provides a preparation method of a nickel-cobalt-manganese ternary material, which aims to improve the tap density of the prepared nickel-cobalt-manganese ternary material, does not influence the electrochemical performance and the cycle performance of the nickel-cobalt-manganese ternary material, and can obtain the nickel-cobalt-manganese ternary material with better performance by performing ball milling processing and spray drying through a ball mill.
The preparation method of the nickel-cobalt-manganese ternary material comprises the following steps:
step one, adding three materials of nickel hydroxide, cobalt hydroxide and manganese carbonate used as raw materials and lithium carbonate used as a lithium source into deionized water to be mixed to obtain a suspension;
step two, adding glucose into the suspension and uniformly stirring to obtain a mixed solution;
and step three, pouring the mixed solution into a ball mill for ball milling to obtain ball milling suspension.
In a specific example, in the first step, 460g of manganese carbonate, 372g of nickel hydroxide, 466.2g of cobalt hydroxide and lithium carbonate (L/M ═ 1.05) are added to 5000g of deionized water, and mixed and stirred for 2 to 6 hours, so as to obtain a uniformly mixed suspension. Here, the mixing in this step means mixing on a physical layer side, and the respective materials do not react with each other. In the second step, the mass of glucose is 1 to 10% of the mass of the raw material, and therefore, 50.1 to 167g of glucose should be added to the suspension and uniformly stirred to obtain a mixed solution, and preferably, when the mass of glucose added to the suspension is 3% of the mass of the raw material, a mixed solution having the best tap density value can be obtained (described in detail later). And in the third step, pouring the mixed solution into a ball mill for ball milling, wherein the rotating speed of the ball mill is 3000-4000 rpm/min, and the ball milling time is 3.5-6 hours, so that the ball milling suspension containing the three raw materials of nickel, cobalt and manganese can be obtained.
Further, the preparation method also comprises the following steps:
and step four, carrying out spray drying on the ball mill processing suspension liquid to carry out primary particle forming, thus obtaining a mixture.
In a specific embodiment, a spray drying apparatus is used in carrying out the spray drying process, the inlet temperature of the spray drying apparatus being 250 ℃ to 290 ℃, and the air flow of the spray drying apparatus being 4m3H to 7m3H is used as the reference value. And the mixture is obtained in a dry state after the spray drying process, and the particle size of the mixture is 1-20 mu m.
Still further, the preparation method further comprises:
and fifthly, placing the mixture in an atmosphere muffle furnace, carrying out secondary particle forming on the mixture under a preset condition, and naturally cooling to obtain the nickel cobalt lithium manganate capable of being used as a battery anode material.
Wherein, in a preferred embodiment, the predetermined conditions include: continuously heating under the air or oxygen atmosphere at a first temperature change value, and raising the temperature in an atmosphere muffle furnace to a first preset temperature for a first preset time; and continuously heating according to a second temperature change value, and raising the temperature in the atmosphere muffle furnace to a second preset temperature for a second preset time. Preferably, the first temperature variation value is 8 ℃/min to 12 ℃/min, the second temperature variation value is 18 ℃/min to 22 ℃/min, the first predetermined temperature is 350 ℃ to 650 ℃, the second predetermined temperature is 850 ℃ to 1000 ℃, the first predetermined time period is 4 hours to 6 hours, and the second predetermined time period is 10 hours to 16 hours. More preferably, the first temperature variation is 10 ℃/min, the first predetermined temperature is 500 ℃, the first predetermined time period is 5 hours, the second temperature variation is 20 ℃/min, the second predetermined temperature is 900 ℃, and the second predetermined time period is 13 hours.
The application also provides a lithium ion battery which comprises an anode, wherein the anode comprises a ternary material, and the ternary material is prepared by adopting the preparation method of the nickel-cobalt-manganese ternary material, so that the tap density of the nickel-cobalt-manganese ternary material is improved, and the electrochemical performance and the use reliability of the lithium ion battery are improved.
In order to verify the electrochemical performance of the nickel-cobalt-manganese ternary material prepared by the preparation method, the nickel-cobalt-manganese lithium prepared by the preparation method, a conductive agent and a binder are mixed according to a certain proportion, then a vacuum ball-milling tank is adopted to perform ball-milling processing for 2 hours at the rotating speed of 600rmp, slurry which is uniformly mixed and has moderate viscosity is prepared to be coated, and vacuum drying is performed to prepare the electrode plate of the positive electrode. The conductive agent adopts super 'P', the diaphragm is celgard 2300, the electrolyte adopts 1mol/L LiPF6 conductive salt and DMC, DEC, EC (wt%) -1: 1:1 solvent, and a proper amount of VC is added into the electrolyte solution as an additive.
After the battery is prepared, the first effect and the cycle performance of the battery are tested under the state of 0.1C, and the charge-discharge cut-off voltage is 2.3V to 4.75V.
By adjusting the mass content of glucose in the preparation method for many times, a relational graph of the tap density of the ternary material and the content of added glucose as shown in fig. 1 can be obtained, and it can be clearly known from the graph that the tap densities of the ternary material are different and are obviously higher than that of a product without added glucose due to different glucose dosages. And further, when the mass content of the glucose accounts for 3% of the mass of the raw materials, the tap density of the ternary material is in the optimal state, and the target requirement can be met.
As can be seen from fig. 2, when the mass of glucose accounts for 3% of the mass of the raw material, the curve of the cycle number and the gram volume of the ternary material prepared by the above method is the same as that of the ternary material without glucose, and the ternary material has good cycle performance, can meet the cycle requirement in the battery charging and discharging process, and ensures the stability and reliability of the battery in the using process.
As shown in fig. 3 and 4, the SEM pictures of the ternary material with glucose added and the mass of glucose added being 3% of the mass of the raw material, and without glucose added. As can be seen from the figure, the shape and the particle size of the particles of the ternary material added with glucose have no obvious change, but the sphericity of the shell of the ternary material can be improved, so that the chemical performance of the ternary material can be improved to a certain extent.
Those skilled in the art will readily appreciate that the above-described preferred embodiments may be freely combined, superimposed, without conflict.
The above is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a nickel-cobalt-manganese ternary material comprises the following steps: adding three materials of nickel hydroxide, cobalt hydroxide and manganese carbonate used as raw materials and lithium carbonate used as a lithium source into deionized water for mixing to obtain a suspension,
the preparation method also comprises the following steps:
adding glucose into the suspension and uniformly stirring to obtain a mixed solution;
and pouring the mixed solution into a ball mill for ball milling to obtain ball milling suspension.
2. The method according to claim 1, wherein the glucose is present in an amount of 1 to 10% by mass based on the mass of the raw material.
3. The method for preparing the nickel-cobalt-manganese ternary material, according to claim 1, wherein the rotation speed of the ball mill is 3000-4000 rpm/min during the ball milling process, and the time of the ball milling process is 3.5-6 hours.
4. The method of claim 1, further comprising the steps of:
and carrying out spray drying on the ball milling suspension to carry out primary particle forming, thus obtaining a mixture.
5. The method for preparing the nickel-cobalt-manganese ternary material according to claim 4, wherein a spray drying apparatus is used in performing the spray drying process,
the inlet temperature of the spray drying equipment is 250 ℃ to 290 ℃; and/or the presence of a gas in the gas,
the air flow of the spray drying equipment is 4m3H to 7m3/h。
6. The method for preparing the nickel-cobalt-manganese ternary material according to claim 4, wherein the particle size of the mixed material is 1-20 μm.
7. The method of preparing a nickel cobalt manganese ternary material of claim 4, further comprising:
and placing the mixture in an atmosphere muffle furnace, carrying out secondary particle forming on the mixture under a preset condition, and naturally cooling to obtain the nickel cobalt lithium manganate capable of being used as a battery anode material.
8. The method of preparing a nickel cobalt manganese ternary material of claim 7, wherein the predetermined conditions include: continuously heating under the air or oxygen atmosphere at a first temperature change value, and raising the temperature in the atmosphere muffle furnace to a first preset temperature for a first preset time;
and continuously heating according to a second temperature change value, and raising the temperature in the atmosphere muffle furnace to a second preset temperature for a second preset time.
9. The method of claim 8, wherein the first temperature variation value is 8 ℃/min to 12 ℃/min; and/or the presence of a gas in the gas,
the second temperature change value is 18 ℃/min to 22 ℃/min; and/or the presence of a gas in the gas,
the first predetermined temperature is 350 ℃ to 650 ℃; and/or the presence of a gas in the gas,
the second predetermined temperature is 850 ℃ to 1000 ℃; and/or the presence of a gas in the gas,
the first predetermined time period is 4 to 6 hours; and/or the presence of a gas in the gas,
the second predetermined period of time is 10 hours to 16 hours.
10. A lithium ion battery comprising a positive electrode, wherein the positive electrode comprises a ternary material prepared by the method of preparing the nickel-cobalt-manganese ternary material according to any one of claims 1 to 9.
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Cited By (1)
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