CN119812235A - Composite negative electrode material, negative electrode, negative electrode preparation method, battery and electrical equipment - Google Patents
Composite negative electrode material, negative electrode, negative electrode preparation method, battery and electrical equipment Download PDFInfo
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Abstract
本申请属于电池技术领域，公开了复合负极材料、负极、负极的制备方法、电池和用电设备。复合负极材料包括负极活性材料、导电剂和预制膜；预制膜包覆在负极活性材料颗粒表面，导电剂分散在预制膜中；预制膜的材料包括聚合物材料。本申请提供的复合负极材料中，预制膜同时包覆在负极活性材料和导电剂表面，利于改善负极活性材料与导电剂的电子传输，降低电极阻抗，提高电池的电化学性能。
The present application belongs to the field of battery technology, and discloses a composite negative electrode material, a negative electrode, a method for preparing a negative electrode, a battery, and an electrical device. The composite negative electrode material includes a negative electrode active material, a conductive agent, and a prefabricated film; the prefabricated film is coated on the surface of the negative electrode active material particles, and the conductive agent is dispersed in the prefabricated film; the material of the prefabricated film includes a polymer material. In the composite negative electrode material provided in the present application, the prefabricated film is coated on the surface of the negative electrode active material and the conductive agent at the same time, which is beneficial to improve the electron transmission between the negative electrode active material and the conductive agent, reduce the electrode impedance, and improve the electrochemical performance of the battery.
Description
Technical Field
The application relates to the technical field of batteries, in particular to a composite negative electrode material, a negative electrode, a preparation method of the negative electrode, a battery and electric equipment.
Background
The cathode materials commonly used in lithium battery production, such as natural/artificial graphite, silica, silicon carbon and the like, can change the volume to a certain extent due to the change of the lattice structure of the cathode materials when undergoing intercalation/alloying reaction with lithium ions, and can cause the thickness change of the cathode and the battery core on a macroscopic scale, thereby bringing challenges to the mechanical design of the battery core and the battery body. In addition, the battery cell can also cause the breakage and regeneration of a natural solid-electrolyte interface (SEI) film due to repeated volume expansion/contraction of a negative electrode material during the operation of the battery cell, and finally, the active lithium loss, the impedance increase and the like are caused to cause failure.
In order to buffer the volume change of the anode material and maintain the stability of the SEI film on the surface of the anode material, a scheme of coating a layer of prefabricated film on the surface of the anode material in advance is proposed and applied, and the prefabricated film is generally a polymer material with a certain elastic modulus and can buffer the volume expansion/contraction of the anode active material in the working process of the battery cell. Then, the polymer material adopted by the existing prefabricated cladding can increase the internal resistance of the electrode and reduce the electrochemical performance of the battery due to the characteristic of no electron conduction.
Disclosure of Invention
The present application aims to solve at least one of the technical problems in the related art to some extent. Therefore, an object of the present application is to provide a composite anode material, an anode, a preparation method of the anode, a battery and electric equipment, wherein in the composite anode material, a prefabricated film is coated on the surfaces of an anode active material and a conductive agent at the same time, which is beneficial to improving electron transmission of the anode active material and the conductive agent, reducing electrode impedance and improving electrochemical performance of the battery.
The first aspect of the application provides a composite anode material. According to an embodiment of the present application, a composite anode material includes an anode active material, a conductive agent, and a prefabricated film, the prefabricated film is coated on the surface of anode active material particles, the conductive agent is dispersed in the prefabricated film, and the material of the prefabricated film includes a polymer material.
In the composite anode material provided by the application, the prefabricated film is coated on the particle surfaces of the anode active material, and the conductive agent is dispersed in the prefabricated film, so that the prefabricated film is coated with the active material and the conductive agent simultaneously, the electron transmission obstruction of the anode active material and the conductive agent is reduced, the electron transmission channel is ensured, the resistance is reduced, and the electrochemical performance of the battery is improved. In addition, unlike common carbon coating processes, the prefabricated film is generally a tough polymer material, can buffer the volume expansion/contraction of the anode active material in the working process of the battery cell, and prolongs the cycle life of the battery cell.
The second aspect of the application provides a negative electrode, which comprises a negative electrode current collector and a negative electrode active material layer, wherein the negative electrode active material layer comprises the composite negative electrode material.
The negative electrode provided by the application comprises the composite negative electrode material, can buffer the volume expansion/contraction of the negative electrode active material in the working process of the battery core, prolongs the cycle life of the battery core, and is beneficial to reducing the electron transmission obstruction of the negative electrode active material and the conductive agent, ensuring the electron transmission channel, reducing the resistance and improving the electrochemical performance of the battery.
The third aspect of the present application provides a method for preparing a negative electrode, comprising:
mixing a negative electrode active material and a conductive agent to obtain a mixed material;
The composite anode material comprises an anode active material, a prefabricated film coated on the surface of anode active material particles and a conductive agent dispersed in the prefabricated film, wherein the prefabricated film is a polymer material formed by polymerization reaction of the monomer material;
mixing the composite anode material with a binder to obtain slurry;
and forming a negative electrode active material layer on the negative electrode current collector by the slurry to obtain a negative electrode.
According to the preparation method of the composite anode material, the prefabricated film is directly prepared in the mixing process of electrode preparation, and no new process and equipment are introduced. And the prefabricated film is coated on the surfaces of the composite anode material and the conductive agent directly in the electrode preparation process, so that the electrode resistance is reduced, and the long cycle life of the battery is prolonged. In addition, the prefabricated film has flexibility, can buffer the volume expansion/contraction of the active material in the working process of the battery cell, and prolongs the cycle life of the battery cell.
In a fourth aspect, the present application provides a battery, which comprises the negative electrode, or the negative electrode prepared by the preparation method.
The battery provided by the application comprises the negative electrode, and has lower resistance and good cycle service life.
In a fifth aspect, the present application provides an electric device, including the battery.
The electric equipment provided by the application comprises the battery. Therefore, the electric equipment has higher safety and good service life.
Additional aspects and advantages of the application will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the application.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
the structure of the composite anode material in the embodiment of the application is shown in fig. 1, wherein the reference numerals in fig. 1 are respectively 1-prefabricated film, 2-anode active material, 3-carbon black and 4-carbon nano tube.
Fig. 2 is a flowchart of a method for manufacturing a negative electrode according to an embodiment of the present application.
Fig. 3 is a flowchart of a method for manufacturing a negative electrode according to an embodiment of the present application.
Fig. 4 is a flowchart of a method for manufacturing a negative electrode according to an embodiment of the present application.
Fig. 5 is a flowchart of a method for manufacturing a negative electrode according to an embodiment of the present application.
Detailed Description
Embodiments of the present application are described in detail below. The following examples are illustrative only and are not to be construed as limiting the application.
It should be noted that the terms "first," "second," and "second" are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implying a number of technical features being indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. Further, in the description of the present application, unless otherwise indicated, the meaning of "a plurality" is two or more.
The endpoints of the ranges and any values disclosed in the present application are not limited to the precise range or value, and the range or value should be understood to include values close to the range or value. For numerical ranges, one or more new numerical ranges may be obtained in combination with each other between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point values, and are to be considered as specifically disclosed in the present application.
In the present application, the terms "comprising" or "including" are used in an open-ended fashion, i.e., to include what is indicated by the present application, but not to exclude other aspects.
At present, in order to buffer the volume change of the anode material and maintain the stability of the SEI film on the surface of the anode material, a scheme of coating a layer of prefabricated film on the surface of the anode material in advance is proposed and applied, and the prefabricated film is generally a polymer material with a certain elastic modulus. However, most of the prefabricated films are applied to the material powder level, and the surface of the anode material is coated with a polymer with poor conductivity, so that electron transmission between the anode material and the conductive agent is blocked, and the impedance of the electrode is increased.
For this purpose, the first aspect of the embodiment of the application provides a composite anode material. According to an embodiment of the present application, a composite anode material includes an anode active material, a conductive agent, and a prefabricated film, the prefabricated film is coated on the surface of anode active material particles, the conductive agent is dispersed in the prefabricated film, and the material of the prefabricated film includes a polymer material.
In the embodiment of the present application, the "conductive agent is dispersed in the prefabricated film", and for any one of the conductive agent particles, it may be entirely or partially located in the prefabricated film, and preferably, most of the conductive agent particles or all of the conductive agent particles are located in the prefabricated film. Taking a combination of carbon black and carbon nano tubes as an example of the conductive agent, the structure of the composite anode material is shown in fig. 1.
In the composite anode material provided by the embodiment of the application, the prefabricated film is coated on the particle surfaces of the anode active material, and the conductive agent is dispersed in the prefabricated film, so that the prefabricated film is coated with the active material and the conductive agent simultaneously, the electron transmission obstruction of the anode active material and the conductive agent is reduced, the electron transmission channel is favorably ensured, the resistance is reduced, and the electrochemical performance of the battery is improved.
In addition, unlike common carbon coating processes, the prefabricated film is generally a tough polymer material, can buffer the volume expansion/contraction of the anode active material in the working process of the battery cell, and prolongs the cycle life of the battery cell.
According to the embodiment of the application, at least one of the following (1) - (3) is satisfied:
(1) The negative electrode active material comprises at least one of graphite, soft carbon, hard carbon, silicon-based material and tin-based material;
(2) The conductive agent comprises at least one of superconductive carbon, acetylene black, carbon black, ketjen black, carbon dots, carbon nanotubes, graphene and carbon nanofibers;
(3) The polymeric material includes an amine-based polymer.
In the present application, the negative electrode active material may employ a negative electrode active material for a battery, which is well known in the art. As an example, the anode active material in the embodiment of the present application may include at least one of graphite, soft carbon, hard carbon, silicon-based material, and tin-based material.
Further, the silicon-based material may include at least one of elemental silicon, a silicon oxygen compound, a silicon carbon compound, a silicon nitrogen compound, and a silicon alloy.
Further, the tin-based material may include at least one of elemental tin, a tin oxide, and a tin alloy.
In the present application, the conductive agent may be a conductive agent for a battery known in the art. As an example, the conductive agent in the embodiment of the present application includes at least one of superconducting carbon, acetylene black, carbon black, ketjen black, carbon dots, carbon nanotubes, graphene, and carbon nanofibers.
In the embodiment of the application, the polymer material comprises an amine polymer, the amine root of the amine polymer contains nitrogen and oxygen elements, and the amine polymer has rich functional groups, can interact with the surface of the anode active material, the binder and the like to strengthen the cohesiveness, is beneficial to improving the structural stability, can effectively buffer the volume expansion/contraction of the anode active material in the working process of the battery cell, and prolongs the cycle life of the battery cell.
According to the embodiment of the application, at least one of the following (1) - (3) is satisfied:
(1) The negative electrode active material includes at least one of graphite and a silicon-based material;
(2) The conductive agent comprises at least one of carbon black and carbon nanotubes;
(3) The polymeric material comprises at least one of polydopamine, polyaniline, and polycaprolactam.
In an embodiment of the present application, the active material substance includes at least one of graphite and a silicon-based material. In practical application, graphite and silicon-based materials show good electrochemical performance and have good market application value, and when the battery cell works, repeated volume expansion/contraction of the negative electrode active materials is easy to cause the breakage of a natural solid-electrolyte interface (SEI) film, and the materials which are easy to expand can be well protected by coating the prefabricated film. Further, the active material includes at least one of graphite, a silicon oxygen compound, and a silicon carbon composite.
In an embodiment of the present application, the conductive agent includes at least one of carbon black and carbon nanotubes. Further, the conductive agent comprises a combination of carbon black and carbon nanotubes, and by dispersing the carbon black and the carbon nanotubes in the prefabricated film, the contact area between the conductive agent and the anode active material is increased, and a good electron transmission path is built.
In an embodiment of the present application, the polymeric material comprises at least one of polydopamine, polyaniline, and polycaprolactam. The polymer has rich functional groups, can interact with the surface of the anode active material, the binder and the like to strengthen the cohesiveness, is beneficial to improving the structural stability, and is convenient to prepare and obtain the polymer with a certain elastic modulus.
According to an embodiment of the present application, the structural formula of the polymer material is shown as formula (I):
The polymer type polydopamine shown in the formula (I) provided by the embodiment of the application has rich imino and hydroxyl groups, has higher electronegativity, and can be adsorbed on the surface of the anode active material through intermolecular force so as to improve the stability of the prefabricated film. When the composite anode material is mixed with a binder to prepare an anode, polydopamine can be crosslinked with the binder to form a network structure, so that the structural stability of the anode is improved.
In the present application, the particle size of the anode active material may be the particle size for a battery, which is well known in the art. The particle size of the conductive agent may be a particle size for a battery, which is well known in the art. In general, the particle size of the conductive agent is smaller than that of the anode active material.
According to an embodiment of the present application, the particle size of the conductive agent is smaller than that of the anode active material, and the conductive agent may be dispersed in the pre-film.
According to the embodiment of the application, at least one of the following (1) - (3) is satisfied:
(1) The average particle diameter of the negative electrode active material is 1-20 mu m;
(2) The average particle size of the conductive agent is 30 nm-100 nm;
(3) The thickness of the prefabricated film is 10 nm-200 nm.
In the embodiment of the present application, the average particle diameter of the anode active material is 1 μm to 20 μm, and in a specific example, the average particle diameter of the anode active material is 1 μm, 3 μm, 5 μm, 7 μm, 9 μm, 11 μm, 13 μm, 15 μm, 17 μm, 19 μm, 20 μm, or the like. The average particle size of the anode active material meets the conditions, which is beneficial to promoting the battery to obtain good charge and discharge performance and cycle stability, and is beneficial to uniformly coating the prefabricated film.
In the embodiment of the application, the average particle size of the conductive agent is 30 nm-100 nm, in a specific example, the average particle size of the conductive agent is 30nm、31nm、32nm、33nm、34nm、35nm、36nm、37nm、38nm、39nm、40nm、41nm、42nm、43nm、44nm、45nm、46nm、47nm、48nm、49nm、50nm、51nm、52nm、53nm、54nm、55nm、56nm、57nm、58nm、59nm、60nm、61nm、62nm、63nm、64nm、65nm、66nm、67nm、68nm、69nm、70nm、71nm、72nm、73nm、74nm、75nm、76nm、77nm、78nm、79nm、80nm、81nm、82nm、83nm、84nm、85nm、86nm、87nm、88nm、89nm、90nm、91nm、92nm、93nm、94nm、95nm、96nm、97nm、98nm、99nm、100nm., and the average particle size of the conductive agent meets the above conditions.
In the embodiment of the application, the thickness of the prefabricated film is 10 nm-200 nm, and in a specific example, the thickness of the prefabricated film is 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 90nm, 100nm, 150nm, 200nm and the like. The conductivity of the polymer material is poor, and the conductivity of the electrode can be influenced after the prefabricated film layer. In the embodiment of the application, the thickness of the prefabricated film meets the conditions, on one hand, a stable structure is obtained, the volume change of the anode material is buffered and not destroyed, and on the other hand, the low internal resistance of the electrode is facilitated, and the long cycle life of the battery is prolonged.
In the embodiment of the application, the average particle size of the anode active material is 1-20 mu m, the average particle size of the conductive agent is 30-100 nm, and the thickness of the prefabricated film is 10-200 nm.
The three components act together to form a uniform and stable preformed film coating layer on the particle surface of the anode active material, and the conductive agent is uniformly dispersed in the preformed film, thereby being beneficial to reducing the electron transmission obstruction, reducing the internal resistance of the electrode and prolonging the cycle service life of the battery.
According to the embodiment of the application, the composite anode material comprises, by weight, 80-96 parts of anode active material, 0.001-2.0 parts of conductive agent and 0.5-3 parts of prefabricated film.
In the embodiment of the application, the dosage of each component in the composite anode material meets the conditions, so that the stable composite anode material is obtained, the electrode resistance is reduced, and the cycle service life of the battery is prolonged. Wherein. The content of the prefabricated film meets the above conditions, and is beneficial to maintaining lower internal resistance of the electrode while ensuring that the prefabricated film provides a good buffering effect for the anode active material.
Further, the prefabricated film is 1-2.5 parts. In specific examples, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2.0 parts, 2.2 parts, 2.4 parts, 2.5 parts, and the like are given.
In the embodiment of the application, the prefabricated film meets the conditions, realizes an effective buffering effect on the anode active material, and simultaneously, effectively coats the anode active material and the conductive agent to reduce the internal resistance of the electrode.
The second aspect of the embodiment of the application provides a negative electrode, which comprises a negative electrode current collector and a negative electrode active material layer, wherein the negative electrode active material layer comprises the composite negative electrode material.
The negative electrode provided by the embodiment of the application comprises the composite negative electrode material, can buffer the volume expansion/contraction of the negative electrode active material in the working process of the battery core, prolongs the cycle life of the battery core, and simultaneously is beneficial to reducing the electron transmission obstruction of the negative electrode active material and the conductive agent, ensuring the electron transmission channel, reducing the resistance and improving the electrochemical performance of the battery.
According to the embodiment of the application, the anode active material layer comprises, by mass, 93% -96% of anode active material, 0.5% -3% of prefabricated film, 0.001% -2.0% of conductive agent and 0.5% -2.5% of binder. In a specific example, the content value of each component is arbitrarily selected within the respective percentage content range, and the sum of the contents of all components is 100%. Wherein, the mass percent of the prefabricated film can be 0.5%, 1%, 0.5%, 1.5%, 2%, 2.5% or 3% and the like.
In the embodiment of the application, the mass percentage of each component meets the conditions, and the components act together to obtain a stable electrode and show good electrochemical performance. The prefabricated film is coated on the surface of the anode active material particles, and the conductive agent is dispersed in the prefabricated film, so that on one hand, an effective buffering effect is provided for the anode active material, and on the other hand, the electronic transmission channel is guaranteed, and the internal resistance of the electrode is reduced. Meanwhile, the preformed film is adsorbed with the binder through the polar group carried by the preformed film to form a stable cross-linked network structure, so that the stability and electrochemical performance of the cathode are further improved.
According to the embodiment of the application, the anode active material layer comprises, by mass, 93% -96% of anode active material, 1% -2.5% of polydopamine, 0.001% -2.0% of conductive agent and 0.5% -2.5% of binder.
In the embodiment of the application, the mass percentage of each component meets the conditions, and the components act together to obtain a stable electrode and show good electrochemical performance.
According to the embodiment of the application, the anode active material layer comprises, by mass, 88% -96% of graphite, 0% -10% of a silicon oxide/silicon carbon compound, 1% -2.5% of polydopamine, 0.001% -2.0% of a conductive agent, and 0.5% -2.5% of a binder.
In the embodiment of the application, the mass percentage of each component meets the conditions, and the components act together, so that the stable electrode can be further obtained, and the electrochemical performance is good.
According to an embodiment of the present application, the negative electrode current collector may employ a current collector conventionally used in the art for batteries. In a specific example, the negative electrode current collector includes a metal foil or a composite current collector. For example, as the metal foil, copper foil may be used. The composite current collector may include a polymeric material base layer and a metal layer formed on at least one surface of the polymeric material base material. The composite current collector may be formed by forming a metal material (copper, copper alloy, nickel alloy, etc.) on a polymer material substrate such as a substrate of polypropylene (PP), polyethylene terephthalate (PET), polybutylene terephthalate (PBT), etc.
In a third aspect of the present application, a method for preparing a negative electrode is provided, including:
mixing a negative electrode active material and a conductive agent to obtain a mixed material;
The composite anode material comprises an anode active material, a prefabricated film coated on the surface of anode active material particles and a conductive agent dispersed in the prefabricated film, wherein the prefabricated film is a polymer material formed by polymerization reaction of the monomer material;
mixing the composite anode material with a binder to obtain slurry;
and forming a negative electrode active material layer on the negative electrode current collector by the slurry to obtain a negative electrode.
In the present application, the term "monomer material" refers to a monomer used for forming a polymer material by polymerization. Auxiliary reagents such as initiators, catalysts, etc. may be added to effect or promote efficient polymer reactions.
In the prior art, the preparation methods of the artificial prefabricated film are applied to the powder level of the anode material, the artificial prefabricated film is coated on the powder level of the anode active material, and then the electrode is prepared, which is not matched with the current cell mass production technology, so that the process steps and the cost are increased. According to the preparation method of the composite anode material, provided by the embodiment of the application, the artificial prefabricated film is directly prepared in the mixing process of electrode preparation, and no new process and equipment are introduced. And the artificial prefabricated film is coated on the surfaces of the composite negative electrode material and the conductive agent directly in the electrode preparation process, so that the electrode resistance is reduced, and the long cycle life of the battery is prolonged. In addition, the artificial prefabricated film has flexibility, can buffer the volume expansion/contraction of the active material in the working process of the battery cell, and prolongs the cycle life of the battery cell.
In a specific example, the preparation method of the negative electrode, as shown in fig. 2, includes the steps of:
s1000, mixing a negative electrode active material and a conductive agent to obtain a mixed material;
s2000, mixing the mixed material with a monomer material to prepare a composite anode material;
s3000, mixing the composite anode material with a binder to obtain slurry;
and S4000, forming a negative electrode active material layer on the negative electrode current collector by the slurry to obtain a negative electrode. After the slurry is coated on the negative electrode current collector, the negative electrode can be further obtained through drying, compacting and cutting.
According to the embodiment of the application, at least one of the following (1) - (3) is satisfied:
(1) The negative electrode active material comprises at least one of graphite, soft carbon, hard carbon, silicon-based material and tin-based material;
(2) The conductive agent comprises at least one of superconductive carbon, acetylene black, carbon black, ketjen black, carbon dots, carbon nanotubes, graphene and carbon nanofibers;
(3) The polymeric material includes an amine-based polymer.
In the present application, the negative electrode active material may employ a negative electrode active material for a battery, which is well known in the art. As an example, the anode active material in the embodiment of the present application may include at least one of graphite, soft carbon, hard carbon, silicon-based material, and tin-based material.
Further, the silicon-based material may include at least one of elemental silicon, a silicon oxygen compound, a silicon carbon compound, a silicon nitrogen compound, and a silicon alloy.
Further, the tin-based material may include at least one of elemental tin, a tin oxide, and a tin alloy.
In the present application, the conductive agent may be a conductive agent for a battery known in the art. As an example, the conductive agent in the embodiment of the present application includes at least one of superconducting carbon, acetylene black, carbon black, ketjen black, carbon dots, carbon nanotubes, graphene, and carbon nanofibers.
In the embodiment of the application, the polymer material comprises an amine polymer, the amine root of the amine polymer contains nitrogen and oxygen elements, and the amine polymer has rich functional groups, can interact with the surface of the anode active material, the binder and the like to strengthen the cohesiveness, is beneficial to improving the structural stability, can effectively buffer the volume expansion/contraction of the anode active material in the working process of the battery cell, and prolongs the cycle life of the battery cell.
According to the embodiment of the application, at least one of the following (1) - (3) is satisfied:
(1) The negative electrode active material includes at least one of graphite and a silicon-based material;
(2) The conductive agent comprises at least one of carbon black and carbon nanotubes;
(3) The polymeric material comprises at least one of polydopamine, polyaniline, and polycaprolactam.
In the embodiment of the application, the active substance comprises at least one of graphite and silicon-based materials, and in practical application, the graphite and silicon-based materials have good electrochemical performance and good market application value. Further, the active material includes at least one of graphite, a silicon oxygen compound, and a silicon carbon composite.
In an embodiment of the present application, the conductive agent includes at least one of carbon black and carbon nanotubes. Further, the conductive agent comprises a combination of carbon black and carbon nanotubes, and by dispersing the carbon black and the carbon nanotubes in the prefabricated film, the contact area between the conductive agent and the anode active material is increased, and a good electron transmission path is built.
In an embodiment of the present application, the polymeric material comprises at least one of polydopamine, polyaniline, and polycaprolactam. The polymer has rich functional groups, can interact with the surface of the anode active material, the binder and the like to strengthen the cohesiveness, is beneficial to improving the structural stability, and is convenient to prepare and obtain the polymer with a certain elastic modulus.
According to an embodiment of the present application, the structural formula of the polymer material is shown as formula (I):
The polymer type polydopamine shown in the formula (I) provided by the embodiment of the application has rich imino and hydroxyl groups, has higher electronegativity, and can be adsorbed on the surface of the anode active material through intermolecular force so as to improve the stability of the prefabricated film. When the composite anode material is mixed with a binder to prepare an anode, polydopamine can be crosslinked with the binder to form a network structure, so that the structural stability of the anode is improved.
In the present application, the particle size of the anode active material may be the particle size for a battery, which is well known in the art. The particle size of the conductive agent may be a particle size for a battery, which is well known in the art. In general, the particle size of the conductive agent is smaller than that of the anode active material.
According to an embodiment of the present application, the particle size of the conductive agent is smaller than that of the anode active material, and the conductive agent may be dispersed in the pre-film.
According to the embodiment of the application, the raw materials adopted in the preparation method comprise, by mass, 93% -96% of anode active material, 1.0% -2.5% of monomer material, 0.001% -2.0% of conductive agent and 0.5% -2.5% of binder. In a specific example, the content value of each component is arbitrarily selected within the respective percentage content range, and the sum of the contents of all components is 100%. Wherein, the mass percent of the prefabricated film can be 0.5%, 1%, 0.5%, 1.5%, 2%, 2.5% or 3% and the like.
In the embodiment of the application, the mass percentage of each component meets the conditions, and the components act together to obtain a stable electrode and show good electrochemical performance. The prefabricated film is coated on the surface of the anode active material particles, and the conductive agent is dispersed in the prefabricated film, so that on one hand, an effective buffering effect is provided for the anode active material, and on the other hand, the electronic transmission channel is guaranteed, and the internal resistance of the electrode is reduced. Meanwhile, the preformed film is adsorbed with the binder through the polar group carried by the preformed film to form a stable cross-linked network structure, so that the stability and electrochemical performance of the cathode are further improved.
According to an embodiment of the application, the monomer material comprises a water-soluble monomer material, preferably the water-soluble monomer material comprises at least one of aniline and dopamine hydrochloride.
In the embodiment of the application, the monomer material is water-soluble monomer material, and can be polymerized in an aqueous solvent environment to form a polymer material of the prefabricated film.
Different from the monomer material of the partially water-insoluble artificial prefabricated film, the embodiment of the application adopts the water-soluble monomer material, is matched with the current negative electrode mixing process, can directly prepare the artificial prefabricated film in the electrode preparation mixing process, and does not introduce new processes, substances and equipment. And water-soluble monomer materials are adopted as raw materials of the prefabricated film, organic solvents are not introduced, and the volatilization risk of toxic solvents and the solvent recovery requirement are avoided.
Further, in an embodiment of the present application, the water-soluble monomer material includes at least one of aniline and dopamine hydrochloride. The water-soluble dopamine monomer is adopted as an artificial SEI material, an organic solvent is not introduced, the volatilization risk of a toxic solvent and the solvent recovery requirement are avoided, and the negative electrode material mixing process can be well matched with the existing negative electrode material mixing process.
According to an embodiment of the present application, a method for preparing a composite anode material includes the steps of:
mixing a negative electrode active material and a conductive agent to obtain a mixed material;
The composite anode material comprises an anode active material, a prefabricated film coated on the surface of anode active material particles and a conductive agent dispersed in the prefabricated film, wherein the prefabricated film is made of polydopamine formed by dopamine hydrochloride through polymerization reaction;
mixing the composite anode material with a binder to obtain slurry;
and forming a negative electrode active material layer on the negative electrode current collector by the slurry to obtain a negative electrode.
In the embodiment of the application, in the step of preparing the composite anode material, dopamine hydrochloride is taken as a monomer material, is a water-soluble monomer, and is directly added with aqueous solution of dopamine hydrochloride in the mixing procedure, correspondingly, the preparation can be completed in an aqueous solvent environment in the mixing procedure of the composite anode material and a binder, and is matched with the existing anode mixing procedure, so that compared with a nonaqueous solvent environment, the preparation method is beneficial to saving cost and simplifying preparation procedure.
In a specific example, the preparation method of the composite anode material, as shown in fig. 3, includes the steps of:
s1000, mixing a negative electrode active material and a conductive agent to obtain a mixed material;
S2000, mixing the mixed material with aqueous solution of dopamine hydrochloride to prepare a composite anode material;
S3000, mixing the composite anode material with an aqueous solution of a binder to obtain slurry;
And S4000, coating the slurry on a negative electrode current collector to form a negative electrode active material layer, so as to obtain the negative electrode.
18. According to the embodiment of the application, in the step of mixing the mixed material with the aqueous solution of dopamine hydrochloride to prepare the composite anode material, tris buffer solution is also added to adjust the pH of the mixed material and the aqueous solution of dopamine hydrochloride.
In the present application, the "Tris buffer" is a buffer prepared from triaminomethane, a salt and distilled water.
In the embodiment of the application, in the step of preparing the composite anode material, tris buffer solution is added for adjusting the pH value of the reaction environment, so that the polymer reaction is promoted to be effectively carried out.
In a specific example, the preparation method of the composite anode material, as shown in fig. 4, includes the steps of:
s1000, mixing a negative electrode active material and a conductive agent to obtain a mixed material;
s2000, mixing the mixed material with aqueous solution of dopamine hydrochloride, and then adding Tris buffer solution to adjust the pH value to prepare a composite anode material;
S3000, mixing the composite anode material with an aqueous solution of a binder to obtain slurry;
And S4000, coating the slurry on a negative electrode current collector to form a negative electrode active material layer, so as to obtain the negative electrode.
In a specific example, the preparation method of the composite anode material, as shown in fig. 5, includes the steps of:
And S1000, mixing the anode active material and the conductive agent to obtain a mixed material. Mechanical stirring and mixing can be used to improve the mixing uniformity. Further, the stirring parameters are controlled to be 10-50 rpm revolution speed, 400-700 rpm autorotation speed and stirring time of 5-20 min.
And S2000, mixing the mixed material with an aqueous solution of dopamine hydrochloride, and then adding a Tris buffer solution to adjust the pH value to prepare the composite anode material. In order to promote the polymerization reaction, the stirring can be carried out under the stirring condition, and further, the stirring parameters are controlled to be 30-80 rpm of revolution speed, 500-800 rpm of rotation speed and 0.5-2 h of stirring time.
And S3000, mixing the composite anode material with an aqueous solution of sodium carboxymethyl cellulose to obtain first slurry. Mechanical stirring and mixing can be used to improve the mixing uniformity. Further, the stirring parameters are controlled to include revolution speed of 30-100 rpm, autorotation speed of 800-2500 rpm and stirring time of 0.5-2 h.
S4000, adding Styrene Butadiene Rubber (SBR) or polyacrylic acid (PAA) and mixing to obtain second slurry. Mechanical stirring and mixing can be used to improve the mixing uniformity. Further, the stirring parameters are controlled to be 10-50 rpm revolution speed, 200-800 rpm autorotation speed and stirring time of 0.5-1 h.
And S5000, coating the second slurry on a negative electrode current collector to obtain a negative electrode.
Further, after step S4000, the second slurry may be taken and tested for solids content and viscosity. The solid content is controlled to be 40% -65%, and the viscosity is controlled to be 800-2500 cp.
According to the embodiment of the application, in the step of preparing the composite anode material by mixing the mixed material with the aqueous solution of dopamine hydrochloride, the control parameters comprise at least one of the following (1) - (3):
(1) The mass concentration of the dopamine hydrochloride is 3% -8%;
(2) The concentration of the Tris buffer solution is 0.05M-0.15M;
(3) And (3) regulating the pH value of the mixed material and the aqueous solution of dopamine hydrochloride to 7.5-9 by using the Tris buffer solution.
In the step of mixing the mixed material with the aqueous solution of dopamine hydrochloride to prepare the composite anode material, the mass concentration of the dopamine hydrochloride is controlled to be 3% -8%, and specific examples are 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5% or 8%. In the embodiment of the application, the mass concentration of the dopamine hydrochloride meets the conditions, which is favorable for promoting the formation of the prefabricated film to form the polydopamine polymer, and the anode active material and the conductive agent are uniformly coated.
Further, the mass concentration of the dopamine hydrochloride is controlled to be 4% -7%, and specific examples are 4%, 4.2%, 4.4%, 4.6%, 4.8%, 5%, 5.2%, 5.4%, 5.6%, 5.8%, 6%, 6.2%, 6.4%, 6.6%, 6.8% or 7%.
In the embodiment of the application, the concentration of the Tris buffer solution is 0.05M-0.15M, and specific examples are 0.05M, 0.07M, 0.09M, 0.1M, 0.11M, 0.13M or 0.15M and the like. In the embodiment of the application, the Tris buffer solution is used for adjusting the pH value of the polymerization reaction and plays a role of an initiator, and the concentration of the Tris buffer solution meets the conditions, so that the polymerization reaction can be effectively promoted to generate a target polydopamine product.
Further, the concentration of Tris buffer was 0.1M.
In the embodiment of the application, the Tris buffer solution adjusts the pH of the mixture and the aqueous solution of dopamine hydrochloride to 7.5-9, and in specific examples, the pH is 7.5, 7.7, 7.9, 8.1, 8.3, 8.5, 8.7, 8.9 or 9. In the embodiment of the application, the polymerization reaction is carried out in a weak alkaline environment, the polymerization efficiency is better, the target polydopamine prefabricated film is formed, and the surfaces of the anode active material and the conductive agent can be uniformly coated.
Further, the Tris buffer solution adjusts the pH of the mixture and the aqueous solution of dopamine hydrochloride to 8-8.5, and specific examples are 8.1, 8.2, 8.3, 8.4 or 8.5.
According to a fourth aspect of the present application, a battery is provided, which includes the above-mentioned negative electrode, or the negative electrode prepared by the above-mentioned preparation method.
The battery provided by the embodiment of the application comprises the negative electrode, and has lower resistance and good cycle service life.
According to an embodiment of the present application, a battery includes a positive electrode sheet, a negative electrode sheet, an electrolyte, and a separator. During the charge and discharge of the battery, active ions are inserted and extracted back and forth between the positive electrode plate and the negative electrode plate. The electrolyte plays a role in conducting ions between the positive electrode sheet and the negative electrode sheet. The isolating film is arranged between the positive plate and the negative plate, and mainly plays a role in preventing the positive plate and the negative plate from being short-circuited, and meanwhile ions can pass through the isolating film.
According to an embodiment of the application, the battery comprises a lithium ion battery or a sodium ion battery.
A fifth aspect of the present application provides an electric device, including the above battery.
The electric equipment provided by the embodiment of the application comprises the battery. Therefore, the electric equipment has higher safety and good service life.
The battery monomer, the battery module and the battery pack can be used as a power supply of electric equipment and also can be used as an energy storage unit of the electric equipment. The powered device may include, but is not limited to, mobile devices (e.g., cell phones, notebook computers, etc.), electric vehicles (e.g., electric only vehicles, hybrid electric vehicles, plug-in hybrid electric vehicles, electric bicycles, electric scooters, electric golf carts, electric trucks, etc.), electric trains, ships and satellites, energy storage systems, and the like.
As the electric device, a battery cell, a battery module or a battery pack may be selected according to the use requirement thereof.
The electric equipment used as one embodiment can be a pure electric vehicle, a hybrid electric vehicle, a plug-in hybrid electric vehicle and the like.
The device as another embodiment may be a mobile phone, a tablet computer, a notebook computer, or the like. The device is generally required to be light and thin, and a battery cell can be used as a power source.
The scheme of the present application will be explained below with reference to examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the present application and should not be construed as limiting the scope of the application. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The embodiment provides a negative electrode plate, which comprises a negative electrode current collector and a negative electrode active material layer, wherein the negative electrode active material layer comprises the components of graphite, silica, carbon black, polydopamine, sodium carboxymethylcellulose (CMC-Na) and Styrene Butadiene Rubber (SBR), and the weight percentages of the components are 91%, 5.0%, 0.8%, 2.0%, 0.6% and 0.6 in sequence. The preparation method comprises the following steps:
and 1, adding a negative electrode active material (graphite and silica) and a conductive agent (carbon black) into a stirring tank for stirring, wherein the revolution speed is 25rpm, the rotation speed is 550rpm, the stirring time is 15min, and the material powder adhered to the wall of the stirring tank is scraped and uniformly stirred.
And 2, adding a dopamine hydrochloride (molecular formula: C 8H12ClNO2) aqueous solution with the mass fraction of 6% into a stirring tank, uniformly mixing, adding a 0.1M Tris buffer solution, adjusting the pH value range of the slurry to 8, continuously stirring to enable dopamine to undergo polymerization reaction, enabling revolution speed to be 50rpm, enabling rotation speed to be 600rpm, and stirring for 1h.
And 3, adding the aqueous solution of sodium carboxymethylcellulose into a stirring tank, continuously stirring, wherein the revolution speed is 60rpm, the rotation speed is 1500rpm, and the stirring time is 1.5h.
And 4, adding Styrene Butadiene Rubber (SBR) into the stirring tank, continuously stirring, wherein the revolution speed is 30rpm, the rotation speed is 500rpm, and the stirring time is 1h.
And 5, slurry sampling test, wherein the solid content is within a range of 40% -65%, and the viscosity is within a range of 800-2500 cp.
And 6, pulping, transferring into a buffer tank, sieving, uniformly coating on a smooth copper foil by a coating machine, and drying by a baking oven to obtain the negative electrode plate.
Preparing a lithium ion battery:
(1) The negative electrode plate is prepared by adopting the embodiment.
(2) The positive electrode plate is prepared by mixing a positive electrode active material LFP (lithium iron phosphate, lithium Iron Phosphate, chemical formula is LiFePO 4), a carbon nano tube and a binder PVDF (polyvinylidene fluoride ) according to the mass ratio of 96%, 1.8% and 2.2%, adding a solvent NMP (N-methyl pyrrolidone, N-methyl-2-pyrrolidone) into a stirring tank, stirring uniformly, coating positive electrode slurry on a smooth aluminum foil, and oven drying.
(3) The preparation of the lithium ion battery comprises the steps of rolling, die cutting, winding, assembling, liquid injection, formation, aging and other standard process flows of the positive electrode plate and the negative electrode plate to obtain the lithium ion battery.
Example 2-example 4
Examples 2 to 4 each provide a negative electrode tab including a negative electrode current collector and a negative electrode active material layer, the composition of the negative electrode active material layer being shown in table 1. Wherein the unit of the component amounts is mass percentage, the binder adopts the combination of CMC-Na and SBR, and the mass ratio of the CMC-Na to the SBR is 1:1.
The specific preparation method of the negative electrode plate is shown in the example 1, and the difference is that the monomer material is replaced by aniline.
The procedure of lithium ion battery was as in example 1.
Table 1 composition of example 2-example 4 electrode active material layers
Example 5-example 9
Examples 5 to 9 each provide a negative electrode tab including a negative electrode current collector and a negative electrode active material layer, the composition of the negative electrode active material layer being as shown in example 1.
The specific preparation method of the negative electrode plate is shown in the embodiment 1, and the difference is that the control parameter values in the step 2 are different, and the specific preparation method is shown in the table 2.
The procedure of lithium ion battery was as in example 1.
Table 2 example 5-example 9 provides process parameters of the negative electrode preparation method
| Sample of | Mass fraction of dopamine hydrochloride | PH value of |
| Example 5 | 3% | 8 |
| Example 6 | 8% | 8 |
| Example 7 | 6% | 7.5 |
| Example 8 | 6% | 8.5 |
| Example 9 | 6% | 9 |
Comparative example 1
The comparative example provides a negative electrode sheet comprising a negative electrode current collector and a negative electrode active material layer, wherein the negative electrode active material layer comprises the components of graphite, silica, carbon black, CMC-Na and SBR, and the components correspond to 91%, 5.0%, 1.8%, 1.1% and 1.1% by weight in sequence.
The specific preparation method of the negative electrode plate is shown in the embodiment 1, and the difference is that the operation of the step 2 is not performed, and the rest steps are the same.
The method of making a lithium ion battery is shown in example 1.
Comparative example 2
The comparative example provides a negative electrode sheet comprising a negative electrode current collector and a negative electrode active material layer, wherein the negative electrode active material layer comprises the components of artificial SEI coated graphite/silica, carbon black, CMC-Na and SBR, and the weight percentages of the components are 98%, 0.8%, 0.6% and 0.6% in sequence.
The specific preparation method of the negative electrode plate is shown in the example 1, and the difference is that:
And 1, dispersing graphite powder, silica and dopamine hydrochloride in deionized water according to a mass ratio of 91:5:2.0, adding a 0.1M Tris buffer solution, adjusting the pH value range of the slurry to 8, and continuously stirring for 1.5h to polymerize the dopamine on the surface of the graphite powder. And sieving and drying the slurry to obtain the prefabricated film coated graphite/silica material.
And 2, coating graphite/silica materials with the prefabricated film, adding the conductive agent (carbon black) into a stirring tank, stirring, wherein the revolution speed is 25rpm, the rotation speed is 550rpm, stirring time is 15min, and scraping and uniformly stirring the material powder attached to the wall of the stirring tank.
And 3, adding CMC-Na water solution into the stirring tank, continuously stirring, wherein the revolution speed is 60rpm, the rotation speed is 1500rpm, and the stirring time is 1.5h.
And 4, adding SBR into the stirring tank to continuously stir, wherein the revolution speed is 30rpm, the rotation speed is 500rpm, and the stirring time is 1h.
And 5, slurry sampling test, wherein the solid content is within a range of 40% -65%, and the viscosity is within a range of 800-2500 cp.
And 6, pulping, transferring into a buffer tank, sieving, uniformly coating on a smooth copper foil by a coating machine, and drying by a baking oven to obtain the negative electrode plate.
The method of making a lithium ion battery is shown in example 1.
Performance testing
1. The testing method comprises the following steps:
1. And (3) membrane resistance test, namely cutting the negative plate into pieces with the thickness of 30mm multiplied by 50mm, peeling the active material layer from the copper foil by using an adhesive tape, and testing the membrane resistance by using a membrane resistance tester.
2. And (3) testing the thickness of the pole piece after circulation: the negative electrode plate is taken out after the cycle of 200 circles of 25 ℃ and 2.2V-3.65V and 0.33C, measuring negative plate thickness with ten thousandth ruler
3 DCIR test 25℃the cell was adjusted to 50% SOC,3C discharged for 10s, and the DC impedance DCIR was calculated.
4. 25 ℃ Cycle test, namely 25 ℃, 2.2V-3.65V, and 1C/1C cycle 1000 circles, and calculating the capacity retention rate.
2. Test results:
TABLE 3 results of Performance test of samples provided by examples and comparative examples
The results of the performance test are shown in Table 3.
The polydopamine is coated on the surface of graphite/silica as a prefabricated film, and the resistance of the coated pole piece is increased compared with that of a non-coated group (comparative example 1) because of the characteristic of no electron conduction, but the resistance of the coated pole piece is slightly increased compared with that of a material particle layer (comparative example 2), and the conductive carbon black is coated on the surface of the anode active material together with the pole piece layer coating (examples 1-9), so that an electron transmission path can be ensured, and the sheet resistance and the direct current resistance are increased slightly compared with those of the non-coated group.
Because the polydopamine can effectively buffer the respiratory expansion of graphite/silica in the circulation process, the thickness increase of the coated pole piece after 1000 circles of circulation is reduced compared with that of the uncoated pole piece, and because the dopamine can be crosslinked with the binder in the polymerization process during pole piece level preparation, the volume expansion after circulation is further limited, and similar expansion inhibition effect can be achieved under the condition of less polydopamine addition (the embodiment 3 and the comparative example 2). Finally, since the respiratory expansion of graphite/silicon oxide during circulation is effectively inhibited by artificial SEI of polydopamine, the fragmentation and regeneration of the original prefabricated film are reduced, and thus the loss of active lithium is reduced, the capacity retention rate of the rest groups after 1000 turns is improved compared with that of comparative example 1, and the capacity retention rate of the pole piece level cladding (examples 1-9) is better than that of the material level cladding (comparative example 2). In conclusion, the cathode coated with the polydopamine prefabricated film at the pole piece level provided by the invention has good comprehensive chemical performance.
While embodiments of the present application have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the application, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the application.
Claims (19)
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