CN109817890B - Preparation method of positive electrode of lithium ion battery - Google Patents
Preparation method of positive electrode of lithium ion battery Download PDFInfo
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- CN109817890B CN109817890B CN201910071933.2A CN201910071933A CN109817890B CN 109817890 B CN109817890 B CN 109817890B CN 201910071933 A CN201910071933 A CN 201910071933A CN 109817890 B CN109817890 B CN 109817890B
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Abstract
The invention belongs to the technical field of batteries, and particularly relates to a preparation method of a lithium ion battery positive electrode. The method comprises the following steps: providing a prefabricated positive electrode, wherein the prefabricated positive electrode comprises a current collector and an active material layer combined on the surface of the current collector, the active material layer comprises a positive active material, a conductive agent and a binder, and the active material layer comprises polyvinylpyrrolidone; extracting the prefabricated positive electrode by using an extracting agent; wherein the polyvinylpyrrolidone is soluble in the extractant. The preparation method can obviously reduce the content of the polyvinylpyrrolidone in the finished product of the positive electrode of the lithium ion battery, thereby reducing the influence of the polyvinylpyrrolidone on the performance of the lithium ion battery, indirectly improving the content of active substances in the pole piece, finally improving the energy density and the cycle performance of the battery, and improving the stability and the applicability of the battery.
Description
Technical Field
The invention belongs to the technical field of batteries, and particularly relates to a preparation method of a lithium ion battery positive electrode.
Background
With the increasing demand for energy density of lithium ion batteries, there are two approaches to improve lithium ion batteries: the unit volume or the unit mass capacity of the active material is improved, and the proportion of the inactive material is reduced as much as possible, so that the proportion of the active material in the battery is indirectly improved. With the development of lithium ion batteries, the application of Carbon Nanotube (CNT) conductive glue solution to the positive electrode of the lithium ion battery as a conductive agent is more and more common, and compared with the traditional conductive agent such as conductive Carbon black conductive agent, the CNT conductive glue solution has the same conductive performance as that of 1/10-1/5 of the conductive Carbon black, so that the dosage of the conductive agent can be obviously reduced, the proportion of active substances is improved, and the energy density of the lithium ion battery is improved.
However, as is well known, the diameter of the carbon nanotube is generally from several nanometers to tens of nanometers, the length of the carbon nanotube is generally from tens of nanometers to hundreds of nanometers, the specific surface area is very high, and the carbon nanotube is easy to agglomerate. The method commonly used in the industry at present is to disperse the CNT in an N-methyl Pyrrolidone solvent, wherein a dispersing agent is polyvinylpyrrolidone (PVP), so as to form a well-dispersed glue solution, the CNT glue solution is directly mixed with a positive electrode material, a solvent and a binder to be pulped when the CNT glue solution is used, and after coating and drying, the polyvinylpyrrolidone is remained in a positive electrode sheet and is finally taken into a lithium ion battery.
Polyvinylpyrrolidone has three main effects in lithium ion batteries: 1. polyvinylpyrrolidone is a non-ionic compound and has no conductivity, so that the energy density of the battery is reduced; 2. under high voltage, the polyvinylpyrrolidone is unstable, is easy to decompose and oxidize, influences the stability of the battery performance, and cannot be used in a voltage system of more than 4.2V; 3. the polyvinylpyrrolidone as a non-conductive substance blocks gaps among pole piece powder, affects the conduction of electrolyte in the pole piece, and affects the rate performance and the cycle performance of the battery.
Therefore, the prior art is in need of improvement.
Disclosure of Invention
The invention aims to provide a preparation method of a lithium ion battery positive electrode, and aims to solve the technical problem that polyvinylpyrrolidone in the conventional lithium ion battery influences the performance of the battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a lithium ion battery positive electrode, which comprises the following steps:
providing a prefabricated positive electrode, wherein the prefabricated positive electrode comprises a current collector and an active material layer combined on the surface of the current collector, the active material layer comprises a positive active material, a conductive agent and a binder, and the active material layer comprises polyvinylpyrrolidone;
extracting the prefabricated positive electrode by using an extracting agent; wherein the polyvinylpyrrolidone is soluble in the extractant.
According to the preparation method of the lithium ion battery positive electrode, after the process of coating slurry to form the prefabricated positive electrode (not finished product), the prefabricated positive electrode is subjected to extraction treatment, and the extractant can dissolve polyvinylpyrrolidone but not other effective components in the extraction process, so that the content of polyvinylpyrrolidone in the finished product of the lithium ion battery positive electrode can be remarkably reduced through the extraction process, the influence of polyvinylpyrrolidone on the performance of the lithium ion battery is reduced, the content of active substances in a pole piece is indirectly increased, the energy density and the cycle performance of the battery are finally improved, and the stability and the applicability of the battery are improved.
Drawings
Fig. 1 is a flow chart of a preparation method of a lithium ion battery positive electrode in the invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In one aspect, an embodiment of the present invention provides a preparation method of a positive electrode of a lithium ion battery, as shown in fig. 1, the preparation method includes the following steps:
s01: providing a prefabricated positive electrode, wherein the prefabricated positive electrode comprises a current collector and an active material layer combined on the surface of the current collector, the active material layer comprises a positive active material, a conductive agent and a binder, and the active material layer comprises polyvinylpyrrolidone;
s02: extracting the prefabricated positive electrode by using an extracting agent; wherein the polyvinylpyrrolidone is soluble in the extractant.
According to the preparation method of the lithium ion battery positive electrode provided by the embodiment of the invention, after the process of coating slurry to form the prefabricated positive electrode (not finished product), the prefabricated positive electrode is subjected to extraction treatment, and the extractant can dissolve polyvinylpyrrolidone but not other effective components in the extraction process, so that the content of polyvinylpyrrolidone in the lithium ion battery positive electrode finished product can be obviously reduced through the extraction process, the influence of polyvinylpyrrolidone on the performance of the lithium ion battery is reduced, the content of active substances in a pole piece is indirectly increased, the energy density and the cycle performance of the battery are finally improved, and the stability and the applicability of the battery are improved.
Specifically, in step S01, the prefabricated positive electrode is an electrode that has not yet been formed into a finished positive electrode for a lithium ion battery, and the general electrode preparation process includes slurry coating, drying, and finally tableting to form a finished positive electrode for a lithium ion battery. The prefabricated positive electrode referred to in the embodiments of the present invention refers to a positive electrode starting product in which a tableting process has not been completed. In one embodiment, the method of making the prefabricated positive electrode comprises: dispersing a positive electrode active material, a conductive agent, a binder and polyvinylpyrrolidone in a solvent to obtain battery positive electrode slurry; and coating the battery positive electrode slurry on the surface of a current collector for drying treatment, namely forming a prefabricated positive electrode. Specifically, taking a carbon nanotube conductive agent as an example, firstly dispersing a carbon nanotube and polyvinylpyrrolidone in a partial solvent to form a uniformly dispersed carbon nanotube glue solution, and then dispersing the carbon nanotube glue solution, a positive electrode active material and a binder in the remaining solvent to obtain a uniformly dispersed battery positive electrode slurry.
Optionally, the positive active material includes one or more of nickel cobalt lithium manganate, lithium cobaltate, lithium iron phosphate and lithium manganate; the binder comprises one or more of polyvinylidene fluoride, carboxymethyl cellulose and styrene butadiene rubber; the conductive agent comprises one or more of carbon nanotubes, acetylene black, Ketjen black, KS-6 and Super P, and preferably the conductive agent is carbon nanotubes. The polyvinylpyrrolidone is used as a dispersant to promote the conductive agent such as the carbon nano tube to form a well-dispersed glue solution, and other dispersants except the polyvinylpyrrolidone can also be added when the battery positive electrode slurry is prepared. The solvent is N-methyl pyrrolidone.
Specifically, in step S02, the extracting agent is at least one selected from a halogenated hydrocarbon extracting agent, an alcohol extracting agent, a nitroalkane extracting agent, a fatty acid extracting agent, and an ester extracting agent. The principle of the extractant is that the extractant has good solubility to polyvinylpyrrolidone, but does not dissolve other effective components, so that the polyvinylpyrrolidone in the active material layer can be effectively released, and other effective substances (such as the positive electrode active material, the conductive agent and the binder) are retained in the active material layer. Specifically, the halogenated hydrocarbon extracting agent is selected from at least one of dichloromethane, dichloroethane, trichloromethane and trichloroethane; the alcohol extractant is selected from at least one of methanol, ethanol, propanol and butanol; the nitroalkane extractant is selected from at least one of nitromethane, nitroethane and nitropropane; the fatty acid extractant is selected from at least one of formic acid, acetic acid and propionic acid; the ester extractant is selected from at least one of ethyl formate, propyl formate, ethyl acetate and methyl acetate. In the embodiment of the invention, ethanol is preferred, and the ethanol extractant is environment-friendly, low in toxicity, low in price and high in practicability.
In one embodiment, the step of subjecting the pre-fabricated positive electrode to an extraction process with an extractant comprises: and placing the prefabricated positive electrode in a device containing the extracting agent for soaking treatment. More preferably, the prefabricated positive electrode is placed in a device containing the extractant which flows circularly, and soaking treatment is carried out. The extraction effect can be improved by the extraction agent which circularly flows. Optionally, the device for containing the extraction is a liquid tank, the liquid tank is provided with a liquid inlet and a liquid outlet, and the liquid inlet and the liquid outlet are communicated, so that a circulating system is formed; the extractant enters the liquid tank through the liquid inlet, and flows through the liquid outlet and the liquid tank, and then flows through the liquid inlet to enter the liquid tank in a circulating manner, so that continuous circulation is carried out, and the extraction effect of the extractant is ensured.
In one embodiment, the prefabricated positive electrode is placed in a device containing the extracting agent, and the soaking treatment is carried out at the temperature T; wherein T is more than or equal to 25 ℃ and less than or equal to the boiling point of the extracting agent. Heating can further improve the extraction efficiency, but the temperature is not too high, and if the temperature is higher than the boiling point of the extracting agent, the extracting agent can be further evaporated, so that in order to ensure the extraction effect, the temperature ranges are as follows: t is more than or equal to 25 ℃ and less than or equal to the boiling point of the extracting agent, and the extraction liquid is heated. In an optional embodiment of the present invention, the extraction agent is ethanol, and the soaking treatment is performed at a temperature of 25 ℃ to 78 ℃; in another optional embodiment of the present invention, the extraction agent is dichloroethane, and the soaking treatment is performed at a temperature of 25 ℃ to 40 ℃; in yet another alternative embodiment of the present invention, the extraction agent is ethyl acetate, and the soaking treatment is performed at a temperature of 25 ℃ to 77 ℃.
In one embodiment, the soaking treatment is performed at a temperature T for 30-60 min. It should be noted that the extractant may be circulated when the preformed positive electrode is placed in the device containing the extractant, and alternatively, the preformed positive electrode may be a continuous transport process in the device, whereby the device containing the extractant has a length such that the preformed positive electrode is in a continuous transport process in the device, and the extractant submerges the preformed positive electrode throughout the process; thus, the soaking time described herein is the time from immersion in the extractant to removal from the device containing the extractant at the same point on the preformed positive electrode.
In one embodiment, after the step of performing the extraction treatment on the prefabricated positive electrode by using the extractant, the step of drying is further included. And drying to evaporate the extractant, and finally tabletting to form the finished product of the lithium ion battery positive electrode. The temperature of the oven is typically greater than the boiling point of the extractant.
In an embodiment of the present invention, a method for preparing a positive electrode of a lithium ion battery includes: (1) dispersing a carbon nano tube conductive agent and polyvinylpyrrolidone in a part of solvent to form uniformly dispersed carbon nano tube glue solution, and then dispersing other substances such as the carbon nano tube glue solution, a positive electrode active material, a binder and the like in the rest solvent to prepare battery positive electrode slurry; (2) coating the battery positive electrode slurry on a current collector, and drying to form a prefabricated positive electrode; (3) placing the prefabricated positive electrode in an extracting agent for an extraction process, and then drying; (4) and (5) preparing the sheet to form the lithium ion battery positive electrode. Compared with the prior art, the preparation method of the lithium ion battery positive electrode provided by the embodiment of the invention adds the process (3), so that the content of polyvinylpyrrolidone in a lithium ion battery positive electrode finished product is obviously reduced, the influence of polyvinylpyrrolidone on the performance of the lithium ion battery is reduced, the content of active substances in a pole piece is indirectly improved, the energy density and the cycle performance of the battery are finally improved, and the stability and the applicability of the battery are improved.
And finally, assembling the prepared positive electrode and the negative electrode of the lithium ion battery to complete liquid injection, and forming a finished battery through activation and formation processes. These are conventional processes and will not be described in detail.
The invention is described in further detail with reference to a part of the test results, which are described in detail below with reference to specific examples.
Example 1
A preparation method of a positive electrode of a lithium ion battery comprises the following steps:
the method comprises the following steps: dispersing a positive electrode active material, a conductive agent, a binder and polyvinylpyrrolidone in a solvent to prepare a battery positive electrode slurry; and coating the battery positive electrode slurry on the surface of a current collector, and drying to form an active material layer to obtain the prefabricated positive electrode.
Step two: and (3) the prefabricated positive electrode formed after coating and drying passes through one or more liquid tanks filled with absolute ethyl alcohol respectively through a guide roller to be extracted. The absolute ethyl alcohol in the liquid tank continuously circulates through the liquid inlet and the liquid outlet respectively to ensure the extraction effect of the absolute ethyl alcohol, and the extraction time is 40 min. In order to ensure the extraction effect, the absolute ethyl alcohol can be heated, and the temperature ranges from room temperature to 78 ℃. The absolute ethyl alcohol has moderate boiling point, environmental protection, low toxicity, low price and strong applicability.
Step three: and after extraction is finished, drying and tabletting to obtain the lithium ion battery positive electrode.
Example 2
A preparation method of a positive electrode of a lithium ion battery comprises the following steps:
the method comprises the following steps: dispersing a positive electrode active material, a conductive agent, a binder and polyvinylpyrrolidone in a solvent to prepare a battery positive electrode slurry; and coating the battery positive electrode slurry on the surface of a current collector, and drying to form an active material layer to obtain the prefabricated positive electrode.
Step two: and the prefabricated positive electrode formed after coating and drying passes through one or more liquid tanks filled with dichloromethane through a guide roller respectively. The dichloromethane in the liquid tank continuously circulates through the liquid inlet and the liquid outlet respectively to ensure the extraction effect of the dichloromethane, and the extraction time is 40 min. To ensure the extraction effect, dichloromethane can be heated to a temperature ranging from room temperature to 40 ℃. The dichloromethane has low boiling point, high toxicity and poor applicability.
Step three: and after extraction is finished, drying and tabletting to obtain the lithium ion battery positive electrode.
Example 3
A preparation method of a positive electrode of a lithium ion battery comprises the following steps:
the method comprises the following steps: dispersing a positive electrode active material, a conductive agent, a binder and polyvinylpyrrolidone in a solvent to prepare a battery positive electrode slurry; and coating the battery positive electrode slurry on the surface of a current collector, and drying to form an active material layer to obtain the prefabricated positive electrode.
Step two: and the prefabricated positive electrode formed after coating and drying passes through one or more liquid tanks filled with ethyl acetate respectively through a guide roller. And the ethyl acetate in the liquid tank continuously circulates through the liquid inlet and the liquid outlet respectively to ensure the extraction effect of the ethyl acetate, and the extraction time is 40 min. To ensure the extraction effect, the ethyl acetate may be heated at a temperature ranging from room temperature to 77 ℃. The ethyl acetate has moderate boiling point, low toxicity, slight irritation and moderate applicability.
Step three: and after extraction is finished, drying and tabletting to obtain the lithium ion battery positive electrode.
Effect testing
The content (mass percentage) of polyvinylpyrrolidone in the positive electrode of the lithium ion battery is tested, and the result is as follows:
TABLE 1
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A preparation method of a positive electrode of a lithium ion battery is characterized by comprising the following steps:
providing a prefabricated positive electrode, wherein the prefabricated positive electrode comprises a current collector and an active material layer combined on the surface of the current collector, the active material layer comprises a positive active material, a conductive agent and a binder, and the active material layer comprises polyvinylpyrrolidone;
extracting the prefabricated positive electrode by using an extracting agent so as to reduce the content of the polyvinylpyrrolidone in the positive electrode of the lithium ion battery; the polyvinylpyrrolidone can be dissolved in the extracting agent, the extracting agent is an ester extracting agent, and the ester extracting agent is at least one selected from ethyl formate, propyl formate, ethyl acetate and methyl acetate.
2. The method of making a lithium ion battery positive electrode of claim 1, wherein the step of subjecting the pre-formed positive electrode to an extraction treatment with an extractant comprises: and placing the prefabricated positive electrode in a device containing the extracting agent for soaking treatment.
3. The method of claim 2, wherein the preformed positive electrode is immersed in a circulating fluid of the extractant in a device.
4. The method for preparing the positive electrode of the lithium ion battery according to claim 2, wherein the prefabricated positive electrode is placed in a device containing the extracting agent, and the soaking treatment is carried out at the temperature T; wherein T is more than or equal to 25 ℃ and less than or equal to the boiling point of the extracting agent.
5. The method for preparing the positive electrode of the lithium ion battery according to claim 4, wherein the extractant is ethyl acetate, and the soaking treatment is performed at a temperature of 25 ℃ to 77 ℃.
6. The method for preparing the positive electrode of the lithium ion battery according to claim 4, wherein the soaking treatment is performed at the temperature T for 30-60 min.
7. The method of making a positive electrode for a lithium-ion battery of any of claims 1-6, wherein the method of making the preformed positive electrode comprises:
dispersing a positive electrode active material, a conductive agent, a binder and polyvinylpyrrolidone in a solvent to obtain battery positive electrode slurry; and coating the battery positive electrode slurry on the surface of a current collector for drying treatment.
8. The method for preparing a positive electrode for a lithium-ion battery according to any of claims 1 to 6, further comprising a step of drying after the step of subjecting the prefabricated positive electrode to an extraction treatment with an extractant.
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