CN114373935B - Negative electrode binder for lithium battery, negative electrode, and lithium battery - Google Patents
Negative electrode binder for lithium battery, negative electrode, and lithium battery Download PDFInfo
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- CN114373935B CN114373935B CN202210112703.8A CN202210112703A CN114373935B CN 114373935 B CN114373935 B CN 114373935B CN 202210112703 A CN202210112703 A CN 202210112703A CN 114373935 B CN114373935 B CN 114373935B
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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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
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 provides a lithium battery negative electrode binder, a negative electrode and a lithium battery, wherein the lithium battery negative electrode binder comprises a block copolymer, the block copolymer comprises a rigid block A and a flexible block B, and the structure of the block copolymer is
Wherein n and m are positive integers, and n is less than or equal to m; the rigid block A is a network cross-linked structure, the flexible block B is a linear structure, and the molecular weight of the block copolymer is 10 4 ～10 7 . According to the invention, through molecular structure design, the block copolymer taking a reticular cross-linked structure rich in polar groups and a flexible long-chain linear structure as main bodies is obtained, the two structures are connected through chemical bonds and are effectively arranged, so that the performance advantages of the two structures are fully exerted, and the block copolymer has the characteristics of high bonding strength, high mechanical strength, high toughness and the like.
Description
Technical Field
The invention relates to the technical field of lithium battery cathodes, in particular to a lithium battery cathode binder, a cathode and a lithium battery.
Background
As the most commonly used binder material for negative electrodes of lithium batteries, CMC-SBR aqueous composite system binders have been studied for decades, but at the same time, the performance of the system reaches the upper limit, and almost no further breakthrough can be made, so that it is difficult to meet the requirement of rapid development of various performances of lithium batteries. The main defects of the CMC-SBR adhesive are that the adhesive capacity is insufficient, the dispersion and the adhesive property to active substances are poor, the integral toughness of the adhesive is poor, the mechanical strength is not high, and a dried adhesive film is easy to break; thus resulting in: (1) the peeling strength of the pole piece is not high, and powder is easy to fall off; (2) The pole piece has poor cracking resistance, and when the coating thickness of the pole piece is increased, the pole piece is easy to crack in the drying process; and (3) the slurry has poor stability and is easy to settle.
In order to overcome the above defects, in recent years, various proposals for replacing CMC-SBR systems, such as polyacrylic acid systems, polyacrylonitrile systems, polyvinyl alcohol systems, polyimide systems, and the like, have been proposed, and have been widely and fully studied in the field of lithium battery negative electrode binders. However, although these systems can improve some performances of the negative electrode, new problems are introduced, such as too strong rigidity of polyacrylic acid system and polyacrylonitrile system, poor thermal performance and mechanical performance of polyvinyl alcohol system, complex polyimide system process, etc., which are still difficult to be widely applied, so that the CMC-SBR system is still the mainstream in the field of negative electrode binders at present.
Disclosure of Invention
The invention provides a lithium battery negative electrode adhesive, a negative electrode and a lithium battery, and aims to solve the technical problems of low peeling strength, poor cracking resistance and poor stability of negative electrode slurry of a negative electrode pole piece in the prior art.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the invention provides a lithium battery negative electrode adhesive which comprises a block copolymer, wherein the block copolymer comprises a rigid block A and a flexible block B, and the structure of the block copolymer is as follows
Wherein n and m are positive integers, and n is less than or equal to m; the rigid block A is a reticular cross-linked structure, the flexible block B is a linear structure, and the molecular weight of the block copolymer is 10 4 ～10 7 。
Further, each of said rigid blocks a is associated with one or more of said flexible blocks B, and/or each of said rigid blocks a is associated with one or more of said rigid blocks a; each of the flexible blocks B is linked to one or more of the rigid blocks A and/or each of the flexible blocks B is linked to one or more of the flexible blocks B.
Further, n is more than or equal to 1 and less than or equal to 10 3 ，10≤m≤10 4 。
Further, the rigid block A has a structural formula:
wherein a, b, c and d are integers between 1 and 5 respectively; r 1 、R 2 、R 3 、R 4 Respectively comprises a cyclic structure, the cyclic structure comprises a hydrocarbon group and a first group, and the first group comprises one or more groups of carbonyl, ester bond, amido bond and ether bond.
Further, the flexible block B has a structural formula as follows:
wherein R is 5 Comprises one or more groups of hydroxyl, carboxyl, ester bond, amido bond and ether bond; r is 6 、R 7 Respectively comprises a linear structure, the linear structure comprises a hydrocarbon group and a second group, and the second group comprises one or more groups of carbonyl, ester bond, amido bond, nitrile group and ether bond.
According to the second aspect of the invention, the lithium battery negative electrode comprises a pole piece coated with negative electrode slurry, and the raw material of the negative electrode slurry comprises the lithium battery negative electrode binder.
According to a third aspect of the present invention, there is also provided a lithium battery including the lithium battery negative electrode described above.
According to the lithium battery cathode adhesive provided by the invention, through the molecular chain structure design, a rigid and polar group-rich net-shaped cross-linking structure is connected with a flexible long-chain linear group through a chemical bond and effectively arranged, so that a rigid and flexible lithium battery cathode adhesive is obtained; the rigid structure endows the adhesive with higher mechanical strength on one hand, and polar groups of the rigid structure have stronger acting force on active substances in the pole piece on the other hand, and the three-dimensional net shape of the rigid structure enables the rigid structure to effectively lift active substance powder; the flexible structure gives the adhesive good flexibility, making it less brittle. Therefore, when the lithium battery cathode adhesive is used for preparing a lithium battery cathode, on one hand, the preparation of cathode slurry with high solid content and difficult sedimentation is facilitated, and on the other hand, the prepared cathode pole piece has high peel strength and is difficult to crack during baking and bending. Therefore, the binder can effectively increase the energy density of the lithium battery.
Drawings
FIG. 1 is a conceptual diagram of a "net-line structure" design of a lithium battery negative binder molecular chain according to an embodiment of the present invention;
FIG. 2 is an EIS curve of batteries fabricated with the negative electrode binders for lithium batteries of examples 1-3 and the comparative CMC-SBR binder;
fig. 3 is a molecular weight distribution curve of a binder of a negative electrode of example 1;
fig. 4 is a DSC curve for the negative electrode binder of example 1;
fig. 5 is a TGA profile of the negative electrode binder of example 1.
Detailed Description
The CMC-SBR aqueous composite system adhesive which is a widely applied lithium battery negative electrode adhesive material has the technical problems of low peeling strength of a negative electrode plate, poor cracking resistance and poor stability of negative electrode slurry. The research shows that the CMC-SBR is a simple blending structure, molecular chains of the two components are only mutually interpenetrated and do not form effective combination and arrangement, so that the advantages of the two components are difficult to effectively exert, namely the good flexibility of the SBR and the acting force of polar groups of the CMC on polar active substances are not fully exerted, and therefore, on a macroscopic scale, the glue film of the CMC-SBR composite adhesive has the characteristics of hard and brittle texture, low mechanical strength, poor adhesive force and the like.
In a first aspect of embodiments of the present application, there is provided a negative electrode binder for a lithium battery, including a block copolymer including a rigid block a and a flexible block B, and having a structure of
Wherein n and m are positive integers, and n is less than or equal to m; the rigid block A forms a network cross-linked structure, the flexible block B forms a linear structure, and the molecular weight of the block copolymer is 10 4 ～10 7 。
Through research, the negative electrode adhesive with a molecular chain in a net-wire structure is designed, and a conceptual diagram is shown in fig. 1. Wherein, the 'net' part is a cross-linked structure rich in polar groups and represents a rigid block A, the 'line' part is a linear long-chain structure and represents a flexible block B, and the 'net' and the 'line' are connected through chemical bonds to finally obtain a three-dimensional molecular structure formed by connecting a plurality of 'spider nets'. Fig. 1 is intended only to illustrate the design concept of the molecular chain structure, and is not intended to represent a molecular chain of a specific configuration.
According to the embodiment of the application, through the molecular structure design, the block copolymer taking the net-shaped cross-linking structure rich in polar groups and the flexible long-chain linear structure as main bodies is obtained, the two structures are connected through chemical bonds and are effectively arranged, so that the performance advantages of the two structures are fully exerted, and the block copolymer has the characteristics of high bonding strength, high mechanical strength, high toughness and the like. The lithium battery negative electrode adhesive is very suitable for the situation of thick coating of a negative electrode plate.
According to the lithium battery cathode adhesive provided by the embodiment of the application, through molecular chain structure design, a rigid and polar group-rich net-shaped cross-linking structure is connected with a flexible long-chain linear group through chemical bonds and effectively arranged, so that a rigid and flexible lithium battery cathode adhesive is obtained; the rigid structure endows the adhesive with higher mechanical strength on one hand, and polar groups of the rigid structure have stronger acting force on active substances in the pole piece on the other hand, and the three-dimensional net shape of the rigid structure enables the rigid structure to effectively lift active substance powder; the flexible structure gives the adhesive good flexibility, making it less brittle. Therefore, when the lithium battery negative electrode binder is used for preparing a lithium battery negative electrode, on one hand, the preparation of negative electrode slurry with high solid content and difficult sedimentation is facilitated, and on the other hand, the prepared negative electrode piece is high in peel strength and difficult to crack during baking and bending. Therefore, the binder can effectively increase the energy density of the lithium battery.
In some embodiments, each rigid block a is linked to one or more flexible blocks B, and/or each rigid block a is linked to one or more rigid blocks a; each flexible block B is linked to one or more rigid blocks A, and/or each flexible block B is linked to a blockAnd a plurality of or more flexible blocks B are connected. In some embodiments, 1 ≦ n ≦ 10 3 ，10≤m≤10 4 。
It is understood that the rigid block a and the flexible block B are chemically linked, by way of non-limiting example, by one or more of a carbon-carbon single bond, an ether linkage, an amide linkage, and an ester linkage.
In some embodiments, the rigid block a has the formula:
wherein a, b, c and d are integers between 1 and 5 respectively; r 1 、R 2 、R 3 、R 4 Respectively comprises a cyclic structure, the cyclic structure comprises a hydrocarbon group and a first group, and the first group comprises one or more groups of carbonyl, ester bond, amido bond and ether bond. Wherein R is 1 、R 2 、R 3 、R 4 Chemical bonds or no chemical bonds are connected between the two groups, and the chemical bonds are represented by dotted lines in the structural formula for the convenience of understanding; as a non-limiting example, when R 1 、R 2 、R 3 、R 4 When the two are connected by a chemical bond, the chemical bond can be one or more of a carbon-carbon single bond, an ether bond, an amido bond and an ester bond.
In some embodiments, the flexible block B has the formula:
wherein R is 5 Comprises one or more groups of hydroxyl, carboxyl, ester bond, amido bond and ether bond; r 6 、R 7 Respectively comprises a linear structure, the linear structure comprises a hydrocarbon group and a second group, and the second group comprises one or more groups of carbonyl, ester bond, amido bond, nitrile group and ether bond.
For the sake of understanding, it is to be noted that the specific structure of the above groups is shown in table 1.
Detailed structural description of the groups in Table 1
It will be appreciated that the rigid block A is linked to the flexible block B by a chemical bond, one end of which is linked to the radical R 1 、R 2 、R 3 、R 4 One end of the other is connected with R 6 、R 7 Any one of them. For ease of understanding, the following structural formula is provided to show one non-limiting example of the manner in which the rigid block A is linked to the flexible block B, where p and q are positive integers.
It is evident that the above structure shows only the connection of one rigid block a and one flexible block B. It will be apparent to those skilled in the art that in other embodiments, each rigid block a may be associated with one or more flexible blocks B, and/or each rigid block a may be associated with one or more rigid blocks a. While each flexible block B may be linked to one or more rigid blocks a and/or each flexible block B is linked to one or more flexible blocks B. In order to effectively form the above-mentioned "network-wire structure", it is obvious that the number n of the rigid blocks A in the molecular chain is not more than the number m of the flexible blocks B, i.e., n.ltoreq.m.
The preparation method of the lithium battery negative electrode binder provided by the embodiment of the application to prepare the lithium battery negative electrode binder comprises the following steps: and (2) carrying out polymerization reaction on a raw material A and a raw material B in a free radical polymerization mode, wherein the raw material A comprises a rigid block A, and the raw material B comprises a flexible block B, and carrying out a batch method or a semi-continuous method to obtain the lithium battery negative electrode binder.
In a second aspect of the embodiments of the present application, there is also provided a lithium battery negative electrode, including a pole piece coated with a negative electrode slurry, where a raw material of the negative electrode slurry includes the above lithium battery negative electrode binder.
Specifically, as a non-limiting example, the preparation method of the negative electrode plate of the lithium battery comprises the following steps: mixing an active substance, a solvent, an auxiliary agent and the lithium battery negative electrode binder to obtain negative electrode slurry; coating the negative electrode slurry on a current collector; and drying the current collector coated with the negative electrode slurry to obtain the negative electrode piece. Wherein the active substance comprises one or more of graphite, silicon carbon and pure silicon. The solvent includes water and/or an organic solvent. The auxiliary agent comprises one or more of a dispersing agent, a thickening agent, a wetting agent, a conductive agent and a defoaming agent.
In a third aspect of the embodiments of the present application, there is also provided a lithium battery including the above lithium battery negative electrode.
The reagents used in the following examples are commercially available.
Example 1
A negative electrode binder for a lithium battery includes a block copolymer, the block copolymer includes a rigid block A and a flexible block B, the rigid block A has a structure formula:
the structural formula of the flexible block B is as follows:
The polymerization method is free radical polymerization, and the polymerization process is a batch method or a semi-continuous method.
Example 2
A lithium battery negative electrode binder comprises a block copolymer, wherein the block copolymer comprises a rigid block A and a flexible block B, and the rigid block A has a structural formula:
the structural formula of the flexible block B is as follows:
The polymerization method is free radical polymerization, and the polymerization process is a batch method or a semi-continuous method.
Example 3
A lithium battery negative electrode binder comprises a block copolymer, wherein the block copolymer comprises a rigid block A and a flexible block B, and the rigid block A has a structural formula:
the structural formula of the flexible block B is as follows:
The polymerization method is free radical polymerization, and the polymerization process is a batch method or a semi-continuous method.
Lithium battery negative electrodes were prepared using the lithium battery negative electrode binders of examples 1 to 3 and a commercially available CMC-SBR binder, respectively. The preparation method comprises the following steps: negative electrode slurry with a solid content of 56% was prepared from the lithium battery negative electrode binders of examples 1 to 3 or commercially available CMC-SBR binders as binder raw materials, copper foils as current collectors, graphite as an active material, acetylene black as a conductive agent, and necessary solvents and auxiliary agents, respectively, and an areal density of 18mg/cm was prepared 2 And then testing. And (3) respectively manufacturing button cells by using the negative pole pieces and testing.
The molecular weight distribution curve of the negative electrode binder of example 1 is shown in fig. 3. Example 1 DSC curve of negative electrode binder referring to fig. 4, it can be seen from fig. 4 that the binder exhibits glass transition behavior at-37.5 ℃, which is characteristic of the flexible block B; the glass transition behaviour of the rigid block A is then not observed in the test temperature range, indicating a temperature higher than 200 ℃. The TGA profile of the negative electrode binder of example 1 is shown in fig. 5. As can be seen from fig. 5, the adhesive began to exhibit a significant thermal weight loss behavior when the test temperature reached about 300 ℃.
The negative electrode paste test results are referenced in table 2, wherein the cell impedance results are referenced in table 2. Fig. 2 shows EIS curves of batteries fabricated with the negative electrode binders for lithium batteries of examples 1 to 3 and the comparative example CMC-SBR binder. As can be seen from fig. 2, the impedance of the batteries corresponding to examples 1 to 3 was lower than that of the battery corresponding to the comparative example.
Table 2 negative electrode paste test results
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of changes or substitutions within the technical scope of the present invention, and all such changes or substitutions are included in the scope of the present invention. Moreover, the technical solutions in the embodiments of the present invention may be combined with each other, but it is necessary to be able to be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent, and is not within the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. A lithium battery negative electrode binder characterized in that: comprises a block copolymer which comprises a rigid block A and a flexible block B and has the structure
Wherein n and m are positive integers, and n is less than or equal to m; the rigid block A is a reticular cross-linked structure, the flexible block B is a linear structure, and the molecular weight of the block copolymer is 10 4 ～10 7 ；
The structural formula of the flexible block B is as follows:
wherein R is 5 Comprises one or more groups of hydroxyl, carboxyl, ester bond, amido bond and ether bond; r 6 、R 7 Respectively comprises a linear structure, the linear structure comprises a hydrocarbon group and a second group, and the second group comprises one or more groups of carbonyl, ester bond, amido bond, nitrile group and ether bond.
2. The negative electrode binder for lithium batteries according to claim 1, wherein each of the rigid blocks a is connected to one or more of the flexible blocks B, and/or each of the rigid blocks a is connected to one or more of the rigid blocks a; each of the flexible blocks B is linked to one or more of the rigid blocks A and/or each of the flexible blocks B is linked to one or more of the flexible blocks B.
3. The negative electrode binder for lithium batteries according to claim 1, wherein n is 1. Ltoreq. N.ltoreq.10 3 ，10≤m≤10 4 。
4. The negative electrode binder for lithium batteries according to any one of claims 1 to 3, wherein the rigid block A has a structural formula of:
wherein a, b, c and d are integers between 1 and 5 respectively; r 1 、R 2 、R 3 、R 4 Respectively comprises a cyclic structure, the cyclic structure comprises a hydrocarbon group and a first group, and the first group comprises one or more groups of carbonyl group, ester bond, amido bond and ether bond.
5. A negative electrode for a lithium battery comprising a pole piece coated with a negative electrode slurry, the raw material of the negative electrode slurry comprising the negative electrode binder for a lithium battery according to any one of claims 1 to 4.
6. A lithium battery comprising the negative electrode for a lithium battery as claimed in claim 5.
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